HCID 178487800、化合物 → HCID 178487794、化合物

HRID 2273204ノート

反応式

HRID 2273204 の反応式
C(O[CH:5]1[C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([O:19][CH3:20])[CH:16]=3)[N:11]=[CH:10][C:9]=2[O:8][CH:7]([O:21][C:22](=[O:24])[CH3:23])[CH:6]1[C@H:25]1[CH2:30][CH2:29][C@H:28]([NH:31][C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:27][CH2:26]1)(=O)C>[Pd].CO>[C:35]([O:34][C:32]([NH:31][C@H:28]1[CH2:27][CH2:26][C@H:25]([CH:6]2[CH2:5][C:18]3[C:17]4[C:12](=[CH:13][CH:14]=[C:15]([O:19][CH3:20])[CH:16]=4)[N:11]=[CH:10][C:9]=3[O:8][CH:7]2[O:21][C:22](=[O:24])[CH3:23])[CH2:30][CH2:29]1)=[O:33])([CH3:38])([CH3:36])[CH3:37]

参加物

4

反応物 1

HCID 178487800HCID 178487800、化合物

生成物 1

HCID 178487794HCID 178487794、化合物収率 71.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

10% Palladium on activated carbon (500 mg, 4.70 mmol, 1.09 eq) is added at room temperature to a stirred solution of acetic acid 4-acetoxy-3-(trans-4-tert-butoxycarbonylamino-cyclo hexyl)-6-methoxy-3,4-dihydro-2H-1-oxa-9-aza-phenanthren-2-yl ester (2.3 g, 4.29 mmol, 1.0 eq) in methanol (60 mL). The reaction mixture is stirred at room temperature under hydrogen flow (10 bars) for 72 hours. The catalyst is then removed by filtration and the solution is concentrated to afford acetic acid 3-(trans-4-tert-butoxycarbonylamino-cyclohexyl)-6-methoxy-3,4-dihydro-2H-1-oxa-9-aza-phenanthren-2-yl ester as a yellow semisolid (1.45 g, 71% yield) which is directly engaged in the next step.

後処理

  1. customThe catalyst is then removed by filtration
  2. concentrationthe solution is concentrated

出典と根拠

ORDレコード
ord-e684fad106ef4540b1fdb396f7666eec
出典データセット
uspto-grants-2015_09
特許番号
US09120822B2

反応ノート

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