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Trifluoroacetic acid → HCID 57968603, 화합물

HRID 882773
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HRID 882773 반응식
C(OC([N:8]1[CH2:12][C@H:11]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:10][C@H:9]1[C:20]([N:22]1[CH2:28][CH2:27][CH2:26][N:25]([CH:29]2[CH2:32][CH2:31][CH2:30]2)[CH2:24][CH2:23]1)=[O:21])=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH2:13]([C@H:11]1[CH2:12][NH:8][C@H:9]([C:20]([N:22]2[CH2:28][CH2:27][CH2:26][N:25]([CH:29]3[CH2:32][CH2:31][CH2:30]3)[CH2:24][CH2:23]2)=[O:21])[CH2:10]1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 44599402HCID 44599402, 화합물

생성물 1

HCID 57968603HCID 57968603, 화합물수율 98.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of (2S,4R)-4-benzyl-2-(4-cyclobutyl-[1,4]diazepane-1-carbonyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (350.8 mg, 0.794 mmol) in CH2Cl2 (2 mL) was treated with TFA (0.5 mL). After 16 h, the mixture was concentrated and the residue was purified by FCC(CH2Cl2 to 10% MeOH/0.1% NH4OH in CH2Cl2) to give the title compound (266.3 mg, 98%). MS (ESI): mass calcd. for C21H31N3O, 341.25; m/z found, 342.3 [M+H]+. 1H NMR (CDCl3): 7.35-7.29 (m, 2H), 7.28-7.22 (m, 1H), 7.16 (d, J=7.9 Hz, 2H), 4.91-4.80 (m, 1H), 4.03-3.38 (m, 4H), 3.20-2.90 (m, 2H), 2.85-2.33 (m, 7H), 2.25-1.56 (m, 11H).

후처리

  1. concentrationthe mixture was concentrated
  2. customthe residue was purified by FCC(CH2Cl2 to 10% MeOH/0.1% NH4OH in CH2Cl2)

출처 및 근거

ORD 기록
ord-d81e56eaacfd468aa033c7f66455dd08
출처 데이터셋
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08236792B2

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