Triethylamine → Methyl 3-[2-[2-(5-methyl-2-thienyl)ethoxy]ethylaminosulphonyl]propanoate

HRID 1422277ノート

反応式

HRID 1422277 の反応式
[CH3:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH2:12])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl[S:21]([CH2:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])(=[O:23])=[O:22]>ClCCl>[CH3:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH:12][S:21]([CH2:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])(=[O:23])=[O:22])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 4962888Methyl 3-(chlorosulfonyl)propanoateHCID 195934942-[2-(5-Methyl-2-thienyl)ethoxy]ethanamine

生成物 1

HCID 18779053Methyl 3-[2-[2-(5-methyl-2-thienyl)ethoxy]ethylaminosulphonyl]propanoate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

The product of step c) as the hydrochloride salt (1.50 g) was stirred under nitrogen in dichloromethane (25 ml). Triethylamine (2.21 ml) was added followed by methyl 3-(chlorosulphonyl)propanoate (1.18 g). The mixture was stirred at room temperature overnight. The solution was diluted with a further amount of dichloromethane and the organics washed with dilute hydrochloric acid then water, then dried (MgSO4). The mixture was filtered and the volatiles removed in vacuo to give the subtitle compound as an oil (1.4 g).

後処理

  1. washthe organics washed with dilute hydrochloric acid
  2. dry with materialwater, then dried (MgSO4)
  3. filtrationThe mixture was filtered
  4. customthe volatiles removed in vacuo

出典と根拠

ORDレコード
ord-85def47d92df43e882d58caea34ba83d
出典データセット
uspto-grants-2000_06
特許番号
US06080869

反応ノート

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