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

HRID 1878432노트

반응식

HRID 1878432 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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]+

후처리

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

출처 및 근거

ORD 기록
ord-a9ecb08071a7420dbb65157065e13031
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314091B2

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