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Benzoyl chloride, 3-chloro- → 4-(3-Chloro-benzoyl)-2,2-dimethyl-piperazine-1-carboxylic acid benzyl ester

HRID 334022
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HRID 334022 반응식
FC(F)(F)C(O)=O.[CH2:8]([O:15][C:16]([N:18]1[CH2:23][CH2:22][NH:21][CH2:20][C:19]1([CH3:25])[CH3:24])=[O:17])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.CCN(C(C)C)C(C)C.[Cl:35][C:36]1[CH:37]=[C:38]([CH:42]=[CH:43][CH:44]=1)[C:39](Cl)=[O:40]>CCOC(C)=O>[CH2:8]([O:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:39](=[O:40])[C:38]2[CH:42]=[CH:43][CH:44]=[C:36]([Cl:35])[CH:37]=2)[CH2:20][C:19]1([CH3:25])[CH3:24])=[O:17])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1
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참가 물질

5

반응물 3

HCID 69252Benzoyl chloride, 3-chloro-HCID 81531DiisopropylethylamineHCID 866882432,2-Dimethyl-piperazine-1-carboxylic acid benzyl ester trifluoroacetate

생성물 1

HCID 866882534-(3-Chloro-benzoyl)-2,2-dimethyl-piperazine-1-carboxylic acid benzyl ester

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3.00 g (8.28 mmol) 2,2-dimethyl-piperazine-1-carboxylic acid benzyl ester trifluoroacetate in 50 mL EtOAc was added 3.50 mL (20.3 mmol) DIPEA followed by 1.07 mL (8.28 mmol) 3-chloro-benzoyl chloride dropwise at RT. The reaction mixture was stirred at RT for 1 h. Then the suspension was washed with water. The combined organic phases were dried over sodium sulfate, filtered and concentrated in vacuo.

후처리

  1. washThen the suspension was washed with water
  2. dry with materialThe combined organic phases were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-6e1b24cbfc6143699900dc94895aa397
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883789B2

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