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HCID 131734349, 화합물 → HCID 68322480, 화합물

HRID 1505394
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HRID 1505394 반응식
CC([N:5]([C@@H:9]([C:12]([NH:14][C:15]1[CH:16]=[N:17][C:18]([O:21][C:22]2[CH:27]=[CH:26][C:25]([C:28]#[N:29])=[C:24]([C:30]([CH3:32])=[CH2:31])[CH:23]=2)=[CH:19][CH:20]=1)=[O:13])[CH2:10][CH3:11])[C:6](=[O:8])[O-:7])(C)C>CO.[Pd]>[C:28]([C:25]1[CH:26]=[CH:27][C:22]([O:21][C:18]2[N:17]=[CH:16][C:15]([NH:14][C:12]([C@H:9]([NH:5][C:6](=[O:8])[O:7][C:24]([CH3:30])([CH3:25])[CH3:23])[CH2:10][CH3:11])=[O:13])=[CH:20][CH:19]=2)=[CH:23][C:24]=1[CH:30]([CH3:31])[CH3:32])#[N:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 131734349HCID 131734349, 화합물2회

생성물 1

HCID 68322480HCID 68322480, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To a solution of 1,1-dimethylethyl((1R)-1-{[(6-{[4-cyano-3-(1-methylethenyl)phenyl]oxy}-3-pyridinyl)amino]carbonyl}propyl)carbamate (Intermediate 178, 73 mg) in MeOH (10 mL) was added Pd 10% w/w on activated carbon (14 mg) and the reaction mixture was stirred for 30 minutes under H2 atmosphere (P=1 atm). The catalyst was filtered off and the solvent removed under reduced pressure. The residue was purified by flash chromatography on silica gel (SNAP 10 g) eluting from 75:25 to 40:60 cyclohexane/ethyl acetate affording the title compound (62 mg) as white solid.

후처리

  1. filtrationThe catalyst was filtered off
  2. customthe solvent removed under reduced pressure
  3. customThe residue was purified by flash chromatography on silica gel (SNAP 10 g)
  4. washeluting from 75:25 to 40:60 cyclohexane/ethyl acetate affording the title compound (62 mg) as white solid

출처 및 근거

ORD 기록
ord-392983f0a0b3405b9ed8ab8640b91db1
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216967B2

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