Triethylamine → 3-(chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide

HRID 1878432ノート

反応式

HRID 1878432 の反応式
[Cl:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6](Cl)=[O:7].C(N(CC)CC)C.Cl.[F:20][C:21]1([F:26])[CH2:24][CH:23]([NH2:25])[CH2:22]1>ClCCl>[Cl:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([NH:25][CH:23]1[CH2:24][C:21]([F:26])([F:20])[CH2:22]1)=[O:7]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27333243-(Chloromethyl)benzoyl chlorideHCID 225009573,3-Difluorocyclobutamine hydrochloride

生成物 1

HCID 668783523-(chloromethyl)-N-(3,3-difluorocyclobutyl)benzamide収率 92.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

3-(Chloromethyl)benzoyl chloride (13.93 mmol, 2.63 g) was stirred in dichloromethane (50 ml) at 0° C. Triethylamine (41.8 mmol, 5.81 ml, 4.23 g) and 3,3-difluorocyclobutanamine hydrochloride (13.93 mmol, 2 g) were combined in dichloromethane and added dropwise. The reaction mixture was allowed to warm to room temperature and stir overnight. The reaction mixture was washed with water, dried over sodium sulfate and concentrated under vacuum to afford the title compound (3.33 g). MS (ESI) m/z 260.3 [M+H]+

後処理

  1. additionadded dropwise
  2. washThe reaction mixture was washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-a9ecb08071a7420dbb65157065e13031
出典データセット
uspto-grants-2012_11
特許番号
US08314091B2

反応ノート

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