反応 #4159627
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-a6c27815aeed4675a144eb724dc6fff0表示可能な構造データがありません
C1=CC(=C(C(=C1CN)F)F)F製品情報
(2,3,4-trifluorophenyl)methanamine (CAS 235088-67-2) 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 2777042
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
7 反応 · 7 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-a6c27815aeed4675a144eb724dc6fff0反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-a6c27815aeed4675a144eb724dc6fff0反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1-Ethyl-5-oxo-proline (0.050 g, 0.32 mmol) was dissolved in anhydrous dichloromethane (˜7 ml) and dimethylformamide (1 ml) and to this was added 1-hydroxybenzotriazole (0.052 g, 0.38 mmol), [(2,3,4-trifluorophenyl)methyl]amine (0.103 g, 0.64 mmol), N-ethyl morpholine (0.151 ml, 0.95 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.073 g, 0.38 mmol). The mixture was shaken at room temperature over the weekend. A further aliquot of [(2,3,4-trifluorophenyl)methyl]amine (0.051 g, 0.32 mmol) was added to the mixture and stirring continued for a while longer until HPLC indicated that no further product was forming. The mixture was diluted with 2M aqueous hydrogen chloride (5 ml) and then filtered through a phase separator. The organic layer was then washed with saturated aqueous sodium hydrogen carbonate and again filtered through a phase separator. The organic layer was then evaporated to give the crude product. The crude material was purified by mass-directed automated HPLC to give pure 1-ethyl-5-oxo-N-[(2,3,4-trifluorophenyl)methyl]-prolinamide (0.032 g). stirring was forming filtered through a phase separator The organic layer was then washed with saturated aqueous sodium hydrogen carbonate again filtered through a phase separator The organic layer was then evaporated to give the crude product The crude material was purified
ソース ID: ord-32bd4605d9704d5db573d2d9d2b76e4b反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1-Ethyl-5-oxo-proline (0.050 g, 0.32 mmol) was dissolved in anhydrous dichloromethane (˜7 ml) and dimethylformamide (1 ml) and to this was added 1-hydroxybenzotriazole (0.052 g, 0.38 mmol), [(2,3,4-trifluorophenyl)methyl]amine (0.103 g, 0.64 mmol), N-ethyl morpholine (0.151 ml, 0.95 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.073 g, 0.38 mmol). The mixture was shaken at room temperature over the weekend. A further aliquot of [(2,3,4-trifluorophenyl)methyl]amine (0.051 g, 0.32 mmol) was added to the mixture and stirring continued for a while longer until HPLC indicated that no further product was forming. The mixture was diluted with 2M aqueous hydrogen chloride (5 ml) and then filtered through a phase separator. The organic layer was then washed with saturated aqueous sodium hydrogen carbonate and again filtered through a phase separator. The organic layer was then evaporated to give the crude product. The crude material was purified by mass-directed automated HPLC to give pure 1-ethyl-5-oxo-N-[(2,3,4-trifluorophenyl)methyl]-prolinamide (0.032 g). stirring was forming filtered through a phase separator The organic layer was then washed with saturated aqueous sodium hydrogen carbonate again filtered through a phase separator The organic layer was then evaporated to give the crude product The crude material was purified
ソース ID: ord-32bd4605d9704d5db573d2d9d2b76e4b反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1-Ethyl-5-oxo-proline (0.050 g, 0.32 mmol) was dissolved in anhydrous dichloromethane (˜7 ml) and dimethylformamide (1 ml) and to this was added 1-hydroxybenzotriazole (0.052 g, 0.38 mmol), [(2,3,4-trifluorophenyl)methyl]amine (0.103 g, 0.64 mmol), N-ethyl morpholine (0.151 ml, 0.95 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.073 g, 0.38 mmol). The mixture was shaken at room temperature over the weekend. A further aliquot of [(2,3,4-trifluorophenyl)methyl]amine (0.051 g, 0.32 mmol) was added to the mixture and stirring continued for a while longer until HPLC indicated that no further product was forming. The mixture was diluted with 2M aqueous hydrogen chloride (5 ml) and then filtered through a phase separator. The organic layer was then washed with saturated aqueous sodium hydrogen carbonate and again filtered through a phase separator. The organic layer was then evaporated to give the crude product. The crude material was purified by mass-directed automated HPLC to give pure 1-ethyl-5-oxo-N-[(2,3,4-trifluorophenyl)methyl]-prolinamide (0.032 g). stirring was forming filtered through a phase separator The organic layer was then washed with saturated aqueous sodium hydrogen carbonate again filtered through a phase separator The organic layer was then evaporated to give the crude product The crude material was purified
ソース ID: ord-9e915935638440ae85ec891ffaf87990反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1-Ethyl-5-oxo-proline (0.050 g, 0.32 mmol) was dissolved in anhydrous dichloromethane (˜7 ml) and dimethylformamide (1 ml) and to this was added 1-hydroxybenzotriazole (0.052 g, 0.38 mmol), [(2,3,4-trifluorophenyl)methyl]amine (0.103 g, 0.64 mmol), N-ethyl morpholine (0.151 ml, 0.95 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.073 g, 0.38 mmol). The mixture was shaken at room temperature over the weekend. A further aliquot of [(2,3,4-trifluorophenyl)methyl]amine (0.051 g, 0.32 mmol) was added to the mixture and stirring continued for a while longer until HPLC indicated that no further product was forming. The mixture was diluted with 2M aqueous hydrogen chloride (5 ml) and then filtered through a phase separator. The organic layer was then washed with saturated aqueous sodium hydrogen carbonate and again filtered through a phase separator. The organic layer was then evaporated to give the crude product. The crude material was purified by mass-directed automated HPLC to give pure 1-ethyl-5-oxo-N-[(2,3,4-trifluorophenyl)methyl]-prolinamide (0.032 g). stirring was forming filtered through a phase separator The organic layer was then washed with saturated aqueous sodium hydrogen carbonate again filtered through a phase separator The organic layer was then evaporated to give the crude product The crude material was purified
ソース ID: ord-9e915935638440ae85ec891ffaf87990反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: 1-Ethyl-5-oxo-proline (0.050 g, 0.32 mmol) was dissolved in anhydrous dichloromethane (˜7 ml) and dimethylformamide (1 ml) and to this was added 1-hydroxybenzotriazole (0.052 g, 0.38 mmol), [(2,3,4-trifluorophenyl)methyl]amine (0.103 g, 0.64 mmol), N-ethyl morpholine (0.151 ml, 0.95 mmol) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (0.073 g, 0.38 mmol). The mixture was shaken at room temperature over the weekend. A further aliquot of [(2,3,4-trifluorophenyl)methyl]amine (0.051 g, 0.32 mmol) was added to the mixture and stirring continued for a while longer until HPLC indicated that no further product was forming. The mixture was diluted with 2M aqueous hydrogen chloride (5 ml) and then filtered through a phase separator. The organic layer was then washed with saturated aqueous sodium hydrogen carbonate and again filtered through a phase separator. The organic layer was then evaporated to give the crude product. The crude material was purified by mass-directed automated HPLC to give pure 1-ethyl-5-oxo-N-[(2,3,4-trifluorophenyl)methyl]-prolinamide (0.032 g). stirring was forming filtered through a phase separator The organic layer was then washed with saturated aqueous sodium hydrogen carbonate again filtered through a phase separator The organic layer was then evaporated to give the crude product The crude material was purified
ソース ID: ord-32bd4605d9704d5db573d2d9d2b76e4bPubChem References
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