Chloroacetyl chloride → N-((1-(2-chloroacetyl)piperidin-4-yl)methyl)-3,5-bis(trifluoromethyl)benzamide

HRID 388783노트

반응식

HRID 388783 반응식
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:24])[C:10]2[CH:15]=[C:14]([C:16]([F:19])([F:18])[F:17])[CH:13]=[C:12]([C:20]([F:23])([F:22])[F:21])[CH:11]=2)[CH2:3][CH2:2]1.CCN(C(C)C)C(C)C.[Cl:34][CH2:35][C:36](Cl)=[O:37]>C(Cl)Cl>[Cl:34][CH2:35][C:36]([N:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:24])[C:10]2[CH:11]=[C:12]([C:20]([F:21])([F:22])[F:23])[CH:13]=[C:14]([C:16]([F:18])([F:19])[F:17])[CH:15]=2)[CH2:3][CH2:2]1)=[O:37]

참가 물질

5

반응물 3

HCID 6577Chloroacetyl chlorideHCID 81531DiisopropylethylamineHCID 57993323N-(piperidin-4-ylmethyl)-3,5-bis(trifluoromethyl)benzamide

생성물 1

HCID 57993392N-((1-(2-chloroacetyl)piperidin-4-yl)methyl)-3,5-bis(trifluoromethyl)benzamide수율 82%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of N-(piperidin-4-ylmethyl)-3,5-bis(trifluoromethyl)benzamide (2.0 g, 5.66 mmol) and DIPEA (1.2 mL) in CH2Cl2 (10 mL) was added 2-chloroacetyl chloride (0.64, 5.66 mmol) dropwise, the mixture was stirred overnight. The mixture was washed with water, dried with Na2SO4, filtered, and the solvent was removed in vacuo. The residue was purified by automated flash chromatography to yield the product (2.0 g, 82%).

후처리

  1. washThe mixture was washed with water
  2. dry with materialdried with Na2SO4
  3. filtrationfiltered
  4. customthe solvent was removed in vacuo
  5. customThe residue was purified by automated flash chromatography

출처 및 근거

ORD 기록
ord-a2cce93bdd884a85acfb23711fb7d6a0
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08377968B2

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