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HCID 10300766, 화합물 → HCID 22285667, 화합물

HRID 1168086
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HRID 1168086 반응식
C1(NS([C:8]2[CH:13]=[C:12]([O:14][C:15]3[C:20]([Cl:21])=[CH:19][C:18]([CH2:22][CH:23]4[S:27][C:26](=[O:28])[NH:25][C:24]4=[O:29])=[CH:17][C:16]=3[Cl:30])[CH:11]=[CH:10][C:9]=2[OH:31])(=O)=O)CC1.[H][H].[C:34](OCC)(=O)C.CO>[Pd]>[Cl:30][C:16]1[CH:17]=[C:18]([CH:19]=[C:20]([Cl:21])[C:15]=1[O:14][C:12]1[CH:11]=[CH:10][C:9]([O:31][CH3:34])=[CH:8][CH:13]=1)[CH2:22][CH:23]1[S:27][C:26](=[O:28])[NH:25][C:24]1=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10300766HCID 10300766, 화합물HCID 21584119Ethylacetate methanolHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22285667HCID 22285667, 화합물

시약·촉매·용매 1

HCID 23938Palladium촉매

실험 절차

The title compound of Step C (93 mg) was dissolved in ethyl acetate/methanol (4 ml/2 ml) and then 10% palladium on carbon (70 mg) was added. The reaction mixture was placed on Parr shaker for four hours under 50 psi hydrogen at room temperature. The solution was filtered through diatomaceous earth, and concentrated. The residue was purified by preparative TLC (3% methanol in dichloromethane) to afford the title compound (52 mg) as a solid. MS (APCl−) Calc: 397.0, Found: 396.0 (M−1).

후처리

  1. filtrationThe solution was filtered through diatomaceous earth
  2. concentrationconcentrated
  3. customThe residue was purified by preparative TLC (3% methanol in dichloromethane)

출처 및 근거

ORD 기록
ord-698ce0bc978c4674a182a60c252f8c4c
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06620830B2

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