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Trifluoroacetic acid → (2-Oxo-2,3,4,5-tetrahydro-benzo[e][1,4]diazepin-1-yl)-acetic acid ethyl ester

HRID 1253883
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HRID 1253883 반응식
C(OC([N:8]1[CH2:14][C:13]2[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=2[N:11]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[C:10](=[O:25])[CH2:9]1)=O)(C)(C)C.[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29]>C(Cl)Cl>[F:26][C:27]([F:32])([F:31])[C:28]([OH:30])=[O:29].[CH2:23]([O:22][C:20](=[O:21])[CH2:19][N:11]1[C:12]2[CH:18]=[CH:17][CH:16]=[CH:15][C:13]=2[CH2:14][NH:8][CH2:9][C:10]1=[O:25])[CH3:24]
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참가 물질

5

반응물 2

HCID 6422Trifluoroacetic acid2회HCID 686381191-Ethoxycarbonylmethyl-2-oxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepine-4-carboxylic acid tert-butyl ester

생성물 2

HCID 6422Trifluoroacetic acidHCID 68637366(2-Oxo-2,3,4,5-tetrahydro-benzo[e][1,4]diazepin-1-yl)-acetic acid ethyl ester수율 92%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

To a solution of 1-ethoxycarbonylmethyl-2-oxo-1,2,3,5-tetrahydro-benzo[e][1,4]diazepine-4-carboxylic acid tert-butyl ester (125 mg, 0.36 mmol) in dry DCM (5 mL) was added trifluoroacetic acid (1.08 mL, 3 mL/mmol). The reaction mixture was stirred at r.t. for one hour. After completion of the reaction, as confirmed by TLC, excess of trifluoroacetic acid and DCM were evaporated in vacuo to afford trifluoroacetic acid salt of (2-oxo-2,3,4,5-tetrahydro-benzo[e][1,4]diazepin-1-yl)-acetic acid ethyl ester (119 mg, 92%) as a gummy solid which was used as such without any further purification for the next step.

후처리

  1. customAfter completion of the reaction
  2. customwere evaporated in vacuo

출처 및 근거

ORD 기록
ord-c76f3e050f3a4f9386525b1d067cab76
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08455479B2

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