Diisopropylethylamine → HCID 68005840、化合物

HRID 74482ノート

反応式

HRID 74482 の反応式
Cl[CH:2]([O:8][CH3:9])[CH2:3][Si:4]([CH3:7])([CH3:6])[CH3:5].[Br:10][C:11]1[CH:12]=[CH:13][C:14]2[N:18]=[C:17]([CH:19]([F:21])[F:20])[NH:16][C:15]=2[CH:22]=1.C(N(CC)C(C)C)(C)C>ClCCl>[Br:10][C:11]1[CH:12]=[CH:13][C:14]2[N:18]=[C:17]([CH:19]([F:20])[F:21])[N:16]([CH2:9][O:8][CH2:2][CH2:3][Si:4]([CH3:7])([CH3:6])[CH3:5])[C:15]=2[CH:22]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 647235395-bromo-2-(difluoromethyl)-1H-1,3-benzodiazoleHCID 87805942(2-Chloro-methoxy-ethyl)-trimethyl-silane

生成物 1

HCID 68005840HCID 68005840、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(2-Chloro-methoxy-ethyl)-trimethyl-silane (1.1 ml, 6.4 mmol, 1.5 eq.) was added to an anhydrous dichloromethane solution (22 ml) of 6-bromo-2-difluoromethyl-1H-benzimidazol (1.0 g, 4.27 mmol) and N,N-diisopropyl ethyl amine (1.9 ml, 10.6 mmol, 2.5 eq.). This was stirred at room temperature for 18 hours. The reaction mixture was concentrated. The residue obtained by concentration under reduced pressure was purified by silica gel column chromatography. Thus, 6-bromo-2-difluoromethyl-1-(2-trimethylsilanyl-ethoxymethyl)-1H-benzimidazole was obtained as a yellow solid (1.37 g, 85%).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. customThe residue obtained by concentration under reduced pressure
  3. customwas purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-376e286b8d604fb5ad3897ccec8a0208
出典データセット
uspto-grants-2014_09
特許番号
US08829199B2

反応ノート

読み込み中…