Cyclohexene → HCID 86643845, 화합물

HRID 1640993노트

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HRID 1640993 반응식
[F:1][C:2]1[CH:3]=[C:4]([S:9]([C:12]2[CH:13]=[C:14]3[C:18](=[CH:19][CH:20]=2)[N:17]([C:21]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[N:16]=[C:15]3[NH:40][C:41](=[O:64])[C:42]2[CH:47]=[CH:46][C:45]([N+:48]([O-])=O)=[CH:44][C:43]=2[N:51]([CH:58]2[CH2:63][CH2:62][O:61][CH2:60][CH2:59]2)[C:52](=[O:57])[C:53]([F:56])([F:55])[F:54])(=[O:11])=[O:10])[CH:5]=[C:6]([F:8])[CH:7]=1.C1CCCCC=1>O1CCOCC1.[Pd]>[NH2:48][C:45]1[CH:46]=[CH:47][C:42]([C:41]([NH:40][C:15]2[C:14]3[C:18](=[CH:19][CH:20]=[C:12]([S:9]([C:4]4[CH:5]=[C:6]([F:8])[CH:7]=[C:2]([F:1])[CH:3]=4)(=[O:10])=[O:11])[CH:13]=3)[N:17]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[N:16]=2)=[O:64])=[C:43]([N:51]([CH:58]2[CH2:59][CH2:60][O:61][CH2:62][CH2:63]2)[C:52](=[O:57])[C:53]([F:56])([F:54])[F:55])[CH:44]=1

참가 물질

5

반응물 2

HCID 8079CyclohexeneHCID 86643846HCID 86643846, 화합물

생성물 1

HCID 86643845HCID 86643845, 화합물

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

To a solution of N-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-yl]-4-nitro-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide (4.05 g, 4.5 mmol) in 1,4-dioxane (100 mL) was added cyclohexene (10 mL) and 10% Pd/C (405 mg). The mixture was stirred at 90° C. for 5 hours, filtered and evaporated to dryness. The residue was purified by flash chromatography on silica gel eluting with ethyl acetate/n-hexane 2:1 affording the title compound as white solid (2.9 g).

후처리

  1. filtrationfiltered
  2. customevaporated to dryness
  3. customThe residue was purified by flash chromatography on silica gel eluting with ethyl acetate/n-hexane 2:1 affording the title compound as white solid (2.9 g)

출처 및 근거

ORD 기록
ord-45f0aea8d2f541899284056fbbbc9467
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08114865B2

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