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Triethylamine → HCID 76485058、化合物

HRID 1599669
ノート
印刷プレビュー

反応式

HRID 1599669 の反応式
BrCCCS(Cl)(=O)=O.NCC[CH2:12][CH2:13][S:14]([NH:17][CH2:18][CH:19]1[CH2:23][CH2:22][CH2:21][N:20]1[C:24](=[O:41])[CH:25]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:39])([CH3:38])[CH3:37])[CH2:26][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)(=[O:16])=[O:15].[CH2:42]([N:44](CC)CC)C>ClCCl>[NH2:44][CH2:42][CH2:12][CH2:13][S:14]([NH:17][CH2:18][CH:19]1[CH2:23][CH2:22][CH2:21][N:20]1[C:24](=[O:41])[CH:25]([NH:33][C:34](=[O:40])[O:35][C:36]([CH3:37])([CH3:38])[CH3:39])[CH2:26][C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)(=[O:15])=[O:16]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 2893293-Bromopropane-1-sulfonyl chlorideHCID 67846374HCID 67846374、化合物

生成物 1

HCID 76485058HCID 76485058、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
-10 °C

実験手順

A solution of Part A 3-bromopropyl sulfonyl chloride (1.06 g, 4.8 mmol) in dichloromethane (5 mL) was added dropwise to a cooled (-10° C.) stirred solution of Example 6a, Part B amine (1.05 g, 3.02 mmol) and triethyl amine (1.44 mL, 9.6 mmol) in dichloromethane (15 mL), After a few minutes, a precipitate formed. The suspension was stirred at -10° C. for 2.5 hours, diluted with dichloromethane (35 mL) and washed with 1N HCl solution (2×15 mL). The dichloromethane solution was dried (MgSO4), filtered and the solvent was removed in vacuo. The crude oil was purified on silica gel (Merck, 150 mL) eluting with 50% ethyl acetate in hexane to give title compound as a white foam (1.160 g, 72%).

後処理

  1. waitAfter a few minutes
  2. customa precipitate formed
  3. washwashed with 1N HCl solution (2×15 mL)
  4. dry with materialThe dichloromethane solution was dried (MgSO4)
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo
  7. customThe crude oil was purified on silica gel (Merck, 150 mL)
  8. washeluting with 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ad2514f72cba405ead6c86388790ef77
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05741799

反応ノート

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