反応 #3880159
関連文献 (1)
openreactiondata ↗doi:10.1039/C8SC04228D
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-dec3d7726ddb45dea3db215c5b90173c表示可能な構造データがありません
C(CNC(=O)C(F)(F)F)N製品情報
N-(2-aminoethyl)-2,2,2-trifluoroacetamide (CAS 5458-14-0) product identity, structure identifiers and related reaction data for chemical intermediate research and sourcing review.
想定用途
専門的研究・工業用途限定
データベース ID 229755
安全上の注意
For professional research and industrial use only. Review the supplier safety data sheet before handling.
合成データ
12 反応 · 12 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-dec3d7726ddb45dea3db215c5b90173c反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-bcb08e25252e482e96399cbc76a6702f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N-1-trifluoroacetylethyldiamine (CF3CONH(CH2)2NH2 is prepared by adding ethyltrifluoroacetate (1.2 ml, 10 mmol) dropwise over one hour to a stirred mixture of ethylenediamine (0.6 g; 10 mmol) and triethylamine (1 ml; 7 mmol) in 20 ml methanol. The solution is stirred overnight. After removal of solvents, the reaction mixture is flash chromatographed on silica using 0-25% methanol in dichloromethane. The fractions containing the desired product are pooled and concentrated to give a colorless product. After removal of solvents chromatographed on silica using 0-25% methanol in dichloromethane The fractions containing the desired product concentrated to give a colorless product
ソース ID: ord-f4e1e48998f148e3a25c6c4677e80ea9反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[(2-Azido-2-(2-ethoxycarbonylmethoxy-ethoxy)-ethoxy]-benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088 g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoro-acetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-d8813e71152a4743a85b9a92064c09b4反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-bcb08e25252e482e96399cbc76a6702f反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[2-Azido-2-(2-ethoxycarbonylmethoxy-ethoxy)-ethoxy]-benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088 g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoro-acetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-88f28fff07f040c98a66170ae5efd505反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[2-Azido-2-(2-ethoxycarbonylmethoxy-ethoxy)-ethoxy]-benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088 g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoro-acetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-88f28fff07f040c98a66170ae5efd505反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[2-Azido-2-(2-ethoxycarbonylmethoxyethoxy)ethoxy]benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoroacetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-6b3503c1d9af4a9eb4bfef0735859596反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N-1-trifluoroacetylethyldiamine (CF3CONH(CH2)2NH2 is prepared by adding ethyltrifluoroacetate (1.2 ml, 10 mmol) dropwise over one hour to a stirred mixture of ethylenediamine (0.6 g; 10 mmol) and triethylamine (1 ml; 7 mmol) in 20 ml methanol. The solution is stirred overnight. After removal of solvents, the reaction mixture is flash chromatographed on silica using 0-25% methanol in dichloromethane. The fractions containing the desired product are pooled and concentrated to give a colorless product. After removal of solvents chromatographed on silica using 0-25% methanol in dichloromethane The fractions containing the desired product concentrated to give a colorless product
ソース ID: ord-6219a7713a3e48a4bffa10853959c2a7反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: N-1-trifluoroacetylethyldiamine (CF3CONH(CH2)2NH2 is prepared by adding ethyltrifluoroacetate (1.2 ml, 10 mmol) dropwise over one hour to a stirred mixture of ethylenediamine (0.6 g; 10 mmol) and triethylamine (1 ml; 7 mmol) in 20 ml methanol. The solution is stirred overnight. After removal of solvents, the reaction mixture is flash chromatographed on silica using 0-25% methanol in dichloromethane. The fractions containing the desired product are pooled and concentrated to give a colorless product. After removal of solvents chromatographed on silica using 0-25% methanol in dichloromethane The fractions containing the desired product concentrated to give a colorless product
ソース ID: ord-5a958693f89c4159981a1c414879050d反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[(2-Azido-2-(2-ethoxycarbonylmethoxy-ethoxy)-ethoxy]-benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088 g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoro-acetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-165c036f62a848e282f4de93cb1f7a42反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 3-[2-Azido-2-(2-ethoxycarbonylmethoxy-ethoxy)-ethoxy]-benzoic acid (0.212 g, 0.6 mmol) was stirred with N,N′-disuccinimidyl carbonate (0.184 g, 0.72 mmol) and DMAP (0.088 g, 0.72 mmol) in dry DMF (1 ml) at room temperature. After 10 minutes, trifluoroacetic acid salt of N-(2-amino-ethyl)-2,2,2-trifluoro-acetamide (0.194 g, 0.72 mmol) was added followed by diisopropylethylamine (DIPEA) (0.251 ml, 1.44 mmol). The reaction mixture was then stirred at room temperature for 17 hours. All the solvents were evaporated under reduced pressure and the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml). The aqueous layer was further extracted with DCM (2×25 ml). All the DCM extracts were combined, dried over MgSO4 and evaporated under reduced pressure. The residue was purified by column chromatography (1×20 cm). The title compound, eluted with 1% methanol in DCM, was obtained as an oil (0.255 g, 86.6%). ES-MS, m/z 490.10 (M−1). All the solvents were evaporated under reduced pressure the residues were partitioned between DCM (50 ml) and aqueous NaH2PO4 (1 N, 50 ml) The aqueous layer was further extracted with DCM (2×25 ml) dried over MgSO4 evaporated under reduced pressure The residue was purified by column chromatography (1×20 cm) The title compound, eluted with 1% methanol in DCM
ソース ID: ord-11cd4e0f0d7e4f0e815356b055b6cbedPubChem References
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