反応 #4163736
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-ae139a06147f445382911cbcf187ba70表示可能な構造データがありません
CNCCS(=O)(=O)C製品情報
N-methyl-2-methylsulfonylethanamine (CAS 202198-18-3) 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 3856040
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
11 反応 · 11 文献
反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-ae139a06147f445382911cbcf187ba70反応条件: temp:0.00; pressure:0.00; stir:
ソース ID: ord-ae139a06147f445382911cbcf187ba70反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Following the general procedure of example 1, 3-[1-(ethylsulfonyl)-4-piperidinyl]-5-(3-formylphenyl)-1H-indole-7-carboxamide (42.0 mg, 0.096 mmol), N-methyl-2-(methylsulfonyl)ethanamine (12.0 mg, 0.087 mmol) and NaBH(OAc)3 (58.0 mg, 0.261 mmol) were reacted to give the title compound (15.1 mg, 28.0%). were reacted
ソース ID: ord-f7f5f83770c24e4bbc8cb39239d511ea反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Following the general procedure of example 1, 3-[1-(ethylsulfonyl)-4-piperidinyl]-5-(3-formylphenyl)-1H-indole-7-carboxamide (42.0 mg, 0.096 mmol), N-methyl-2-(methylsulfonyl)ethanamine (12.0 mg, 0.087 mmol) and NaBH(OAc)3 (58.0 mg, 0.261 mmol) were reacted to give the title compound (15.1 mg, 28.0%). were reacted
ソース ID: ord-f7f5f83770c24e4bbc8cb39239d511ea反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In an analogous manner to Example 10, 5-(4-(4-Benzyloxy-phenylamino)-quinazolin-6-yl)-furan-2-carbaldehyde hydrochloride (0.217 g, 0.474 mmol) was reacted with N-methyl-N-(2-methanesulphonyl-ethyl)amine (0.411 g, 3.0 mmol). Purification by silica gel chromatography, eluting with 2-3% MeOH/CHCl3, followed by trituration with ether, gave the title compound as a pale yellow solid (0.100 g, 0.184 mmol, 39%); δH [2H6]DMSO 9.84 (1H, s), 8.63 (1H, s), 8.48 (1H, s), 8.12 (1H, d), 7.78 (1H, d), 7.68 (2H, d), 7.13-7.52 (5H, m), 7.02-7.10 (3H, m), 6.55 (1H, d), 5.14 (2H, s), 3.70 (2H, s), 3.35-3.44 (2H, obscured by water), 3.05 (3H, s), 2.84 (2H, t), 2.28 (3H, s). Purification by silica gel chromatography eluting with 2-3% MeOH/CHCl3
ソース ID: ord-c0ebf79d1c67434ca5c31c56111d353d反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In an analogous manner to Example 10, 5-(4-(4-Benzyloxy-phenylamino)-quinazolin-6-yl)-furan-2-carbaldehyde hydrochloride (0.217 g, 0.474 mmol) was reacted with N-methyl-N-(2-methanesulphonyl-ethyl)amine (0.411 g, 3.0 mmol). Purification by silica gel chromatography, eluting with 2-3% MeOH/CHCl3, followed by trituration with ether, gave the title compound as a pale yellow solid (0.100 g, 0.184 mmol, 39%); δH [2H6]DMSO 9.84 (1H, s), 8.63 (1H, s), 8.48 (1H, s), 8.12 (1H, d), 7.78 (1H, d), 7.68 (2H, d), 7.13-7.52 (5H, m), 7.02-7.10 (3H, m), 6.55 (1H, d), 5.14 (2H, s), 3.70 (2H, s), 3.35-3.44 (2H, obscured by water), 3.05 (3H, s), 2.84 (2H, t), 2.28 (3H, s). Purification by silica gel chromatography eluting with 2-3% MeOH/CHCl3
ソース ID: ord-c0ebf79d1c67434ca5c31c56111d353d反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: (R)-2-(6-Fluoro-3-oxopyrrolo[4,3,2-de][2,6]naphthyridin-4(1H,3H,5H)-yl)-3-methylbutanoic acid (15 mg, 0.051 mmol), HOBt hydrate (9.46 mg, 0.062 mmol), and EDC hydrochloride (14.81 mg, 0.077 mmol) were combined in DMF (2 mL). N-methyl-2-(methylsulfonyl)ethanamine (10.60 mg, 0.077 mmol) and 4-methylmorpholine (0.023 mL, 0.206 mmol) were added, and the reaction mixture was stirred at room temperature for 2 h. The product was purified by preparative HPLC (10-45% AcCN/H2O with 0.035% TFA), concentrated in vacuo, and lyophilized to afford the title compound as a white solid (12 mg, 57% yield). 1H NMR (500 MHz, CD3OD) δ 0.77 (d, J=6.5 Hz, 3H), 0.95 (d, J=6.5 Hz, 3H), 2.41-2.49 (m, 1H), 2.97 (s, 3H), 3.05 (s, 3H), 3.36 (t, J=6.5 Hz, 2H), 3.78 (t, J=6.5 Hz, 2H), 4.81-4.96 (m, 2H), 5.36 (d, J=11.0 Hz, 1H), 7.97 (d, J=2.5 Hz, 1H), 8.23 (d, J=2.5 Hz, 1H), 12.39 (s, 1H). [M+H] calc'd for C18H23FN4O4S, 411; found, 411. The product was purified by preparative HPLC (10-45% AcCN/H2O with 0.035% TFA) concentrated in vacuo
ソース ID: ord-e29652ae719e457d8fd1ac5dd8d4464b反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: In an analogous manner to Example 10, 5-(4-(4-Benzyloxy-phenylamino)-quinazolin-6-yl)-furan-2-carbaldehyde hydrochloride (0.217 g, 0.474 mmol) was reacted with N-methyl-N-(2-methanesulphonyl-ethyl)amine (0.41 1g, 3.0 mmol). Purification by silica gel chromatography, eluting with 2-3% MeOH/CHCl3, followed by trituration with ether, gave the title compound as a pale yellow solid (0.100 g, 0.184 mmol, 39%); δH [2H6]DMSO 9.84 (1H,s), 8.63 (1H,s), 8.48 (1H,s), 8.12 (1H,d), 7.78 (1H,d), 7.68 (2H,d), 7.13-7.52 (5H,m), 7.02-7.10 (3H,m), 6.55 (1H,d), 5.14 (2H,s), 3.70 (2H,s), 3.35-3.44 (2H, obscured by water), 3.05 (3H,s), 2.84 (2H,t), 2.28 (3H,s). Purification by silica gel chromatography eluting with 2-3% MeOH/CHCl3
ソース ID: ord-f306fe2b301b4d62a2ca14eb6b0f29ee反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Following the general procedure of example 1, 3-[1-(ethylsulfonyl)-4-piperidinyl]-5-(3-formylphenyl)-1H-indole-7-carboxamide (42.0 mg, 0.096 mmol), N-methyl-2-(methylsulfonyl)ethanamine (12.0 mg, 0.087 mmol) and NaBH(OAc)3 (58.0 mg, 0.261 mmol) were reacted to give the title compound (15.1 mg, 28.0%). were reacted
ソース ID: ord-7c3ee9df27704347be169b6104da478e反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: (R)-2-(6-Fluoro-3-oxopyrrolo[4,3,2-de][2,6]naphthyridin-4(1H,3H,5H)-yl)-3-methylbutanoic acid (15 mg, 0.051 mmol), HOBt hydrate (9.46 mg, 0.062 mmol), and EDC hydrochloride (14.81 mg, 0.077 mmol) were combined in DMF (2 mL). N-methyl-2-(methylsulfonyl)ethanamine (10.60 mg, 0.077 mmol) and 4-methylmorpholine (0.023 mL, 0.206 mmol) were added, and the reaction mixture was stirred at room temperature for 2 h. The product was purified by preparative HPLC (10-45% AcCN/H2O with 0.035% TFA), concentrated in vacuo, and lyophilized to afford the title compound as a white solid (12 mg, 57% yield). 1H NMR (500 MHz, CD3OD) δ 0.77 (d, J=6.5 Hz, 3H), 0.95 (d, J=6.5 Hz, 3H), 2.41-2.49 (m, 1H), 2.97 (s, 3H), 3.05 (s, 3H), 3.36 (t, J=6.5 Hz, 2H), 3.78 (t, J=6.5 Hz, 2H), 4.81-4.96 (m, 2H), 5.36 (d, J=11.0 Hz, 1H), 7.97 (d, J=2.5 Hz, 1H), 8.23 (d, J=2.5 Hz, 1H), 12.39 (s, 1H). [M+H] calc'd for C18H23FN4O4S, 411; found, 411. The product was purified by preparative HPLC (10-45% AcCN/H2O with 0.035% TFA) concentrated in vacuo
ソース ID: ord-195d36155d98432faaffe58215ddc3d2反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Following the general procedure of example 1, 3-[1-(ethylsulfonyl)-4-piperidinyl]-5-(3-formylphenyl)-1H-indole-7-carboxamide (42.0 mg, 0.096 mmol), N-methyl-2-(methylsulfonyl)ethanamine (12.0 mg, 0.087 mmol) and NaBH(OAc)3 (58.0 mg, 0.261 mmol) were reacted to give the title compound (15.1 mg, 28.0%). were reacted
ソース ID: ord-f7f5f83770c24e4bbc8cb39239d511eaPubChem References
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