3-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-5-acetoxy-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one → 3-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one

HRID 2418743ノート

反応式

HRID 2418743 の反応式
[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:15][CH:14](OC(=O)C)[C:13]2[CH:20]=[CH:21][CH:22]=[CH:23][C:12]=2[N:11]([CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:10]1=[O:32])=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)C.[Pd]>[C:1]([O:5][C:6]([NH:8][C@H:9]1[CH2:15][CH2:14][C:13]2[CH:20]=[CH:21][CH:22]=[CH:23][C:12]=2[N:11]([CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:10]1=[O:32])=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 1

HCID 132435333-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-5-acetoxy-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one

生成物 1

HCID 132435313-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A solution of 3-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-5-acetoxy-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one (2.2 g) in ethanol (300 ml) containing 10% Pd/C (2.0 g) was placed in a pressure bottle and hydrogenated at 3 atmospheres pressure and 70° for 3 days. The catalyst was filtered off and the filtrate evaporated to give 3-(S)-t-butyloxycarbonylamino-1-t-butyloxycarbonylmethyl-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, m.p. 164°-165° [α]D =-200.6° (c=0.64 in DMF).

後処理

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate evaporated

出典と根拠

ORDレコード
ord-643046da9cf048d6b7487070b909cda6
出典データセット
uspto-grants-1984_09
特許番号
US04473575

反応ノート

読み込み中…