Triethylamine → HCID 67973483、化合物

HRID 925303ノート

反応式

HRID 925303 の反応式
C(N(CC)CC)C.Cl.[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[NH:15][CH:14]=[C:13]2[CH2:19][CH2:20][NH2:21].[I:22][C:23]1[CH:31]=[CH:30][C:26]([C:27](Cl)=[O:28])=[CH:25][CH:24]=1>ClCCl>[Cl:9][C:10]1[CH:11]=[C:12]2[C:16](=[CH:17][CH:18]=1)[NH:15][CH:14]=[C:13]2[CH2:19][CH2:20][NH:21][C:27](=[O:28])[C:26]1[CH:30]=[CH:31][C:23]([I:22])=[CH:24][CH:25]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 743734-Iodobenzoyl chlorideHCID 28274945-Chloro-1H-indole-3-ethylamine monohydrochloride

生成物 1

HCID 67973483HCID 67973483、化合物収率 45.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-(2-(5-chloro-1H-indol-3-yl)ethyl)-4-iodobenzamide was prepared according to method C with triethylamine (2.23 mL; 15.90 mmol), 2-(5-chloro-1H-indol-3-yl)ethanamine hydrochloride (1.5 g; 6.36 mmol) and 4-iodobenzoyl chloride (1.82 g; 6.68 mmol) in dichloromethane (75 mL). The mixture was stirred for 20 minutes at room temperature and was evaporated under reduced pressure. The crude material was purified by flash chromatography on silica gel (eluent 2 to 20% ethyl acetate in dichloromethane) to provide 1.22 g (45%) of N-(2-(5-chloro-1H-indol-3-yl)ethyl)-4-iodobenzamide as a white solid.

後処理

  1. customN-(2-(5-chloro-1H-indol-3-yl)ethyl)-4-iodobenzamide was prepared
  2. customwas evaporated under reduced pressure
  3. customThe crude material was purified by flash chromatography on silica gel (eluent 2 to 20% ethyl acetate in dichloromethane)

出典と根拠

ORDレコード
ord-8f064a51dbf748e799231cf56ec51dd6
出典データセット
uspto-grants-2016_03
特許番号
US09284271B2

反応ノート

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