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HCID 54257403, 화합물 → HCID 9909040, 화합물

HRID 1017552
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HRID 1017552 반응식
C([O:8][C:9](=[O:35])[CH2:10][CH:11]([S:19]([N:22]1[CH2:27][CH2:26][CH:25]([CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH2:24][CH2:23]1)(=[O:21])=[O:20])[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)C1C=CC=CC=1>CCOC(C)=O.[Pd]>[CH2:28]([CH:25]1[CH2:26][CH2:27][N:22]([S:19]([CH:11]([CH2:12][C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH2:10][C:9]([OH:35])=[O:8])(=[O:21])=[O:20])[CH2:23][CH2:24]1)[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 54257403HCID 54257403, 화합물

생성물 1

HCID 9909040HCID 9909040, 화합물수율 99.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8857Ethyl Acetate용매

실험 절차

The product from Step E (360 mg, 0.73 mmol) was taken up in EtOAc (10 mL) with stirring under a blanket of argon. 10% palladium on charcoal (130 mg) was added. The resulting suspension was hydrogenated in a PARR apparatus at room temperature overnight. The system was purged with argon and the catalyst removed by filtration. The filtrate was evaporated under reduced pressure to give the desired product as a gum (292mg, Quant). 1H-NMR δ(MeOD) 7.24-7.10 (10H, m), 3.89 (1H, m), 3.69 (2H, m), 3.25 (1H, dd, J=4.8, 17.1 Hz), 2.81-2.64 (4H, m), 2.53 (2H, d, J=6.7 Hz), 2.45 (1H, dd, J=4.8, 17.1 Hz), 1.61 (3H, m) and 1.28 (2H, m). 13C-NMR δ(MeOD) 174.3, 141.7, 138.8, 130.8, 130.6, 130.2, 129.7, 128.4, 127.4, 61.0, 47.6, 44.2, 39.2, 36.6, 34.8, 33.7. ESMS=(M+1) 402.2, (M−1) 400.0.

후처리

  1. customThe system was purged with argon
  2. customthe catalyst removed by filtration
  3. customThe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-98a059af2ca34587a8a8154bcca6c3df
출처 데이터셋
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06479502B1

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