Cyclohexene → HCID 86643845、化合物

HRID 1640993ノート

反応式

HRID 1640993 の反応式
[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

参加物

5

反応物 2

HCID 8079CyclohexeneHCID 86643846HCID 86643846、化合物

生成物 1

HCID 86643845HCID 86643845、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
90 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-45f0aea8d2f541899284056fbbbc9467
出典データセット
uspto-grants-2012_02
特許番号
US08114865B2

反応ノート

読み込み中…