HCID 15051736、化合物 → HCID 15051737、化合物

HRID 1252447ノート

反応式

HRID 1252447 の反応式
[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH:38]([O:41][CH3:42])[O:39][CH3:40])[CH:8]=[C:9]2[C:17]=1[CH:16]([CH2:18][O:19][C:20](=[O:22])[NH2:21])[C:15]1([O:24][C:25](=[O:27])[CH3:26])[O:23][N:10]2[CH2:11][CH:12]2[CH:14]1[N:13]2C(OCC1C=CC=CC=1)=O)(=[O:3])[CH3:2]>CO.[Pd]>[C:1]([O:4][C:5]1[CH:6]=[C:7]([CH:38]([O:39][CH3:40])[O:41][CH3:42])[CH:8]=[C:9]2[C:17]=1[CH:16]([CH2:18][O:19][C:20](=[O:22])[NH2:21])[C:15]1([O:24][C:25](=[O:27])[CH3:26])[O:23][N:10]2[CH2:11][CH:12]2[CH:14]1[NH:13]2)(=[O:3])[CH3:2]

参加物

4

反応物 1

HCID 15051736HCID 15051736、化合物

生成物 1

HCID 15051737HCID 15051737、化合物収率 40.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of 11-benzyloxycarbonyl-8-carbamoyloxymethyl-4-dimethoxymethyl-14-oxa-1,11-diazatetracyclo[7.4.1.02,7.010,12 ]tetradeca-2,4,6-trien-6,9-diyl diacetate (100 mg) in methanol (10 ml) was added 10% palladium on carbon (50 mg). The mixture was stirred for 1 hour under hydrogen atmosphere (20 psi) at ambient temperature. The reaction mixture was filtered through cellulose powder and the filtrate was evaporated in vacuo. The residue was subjected to preparative thin layer chromatography, which was developed with a mixture of chloroform and methanol (10:1, v/v) to afford A-isomer of 8-carbamoyloxymethyl-4-dimethoxymethyl-14-oxa-1,11-diazatetracyclo[7.4.1.02,7.010,12 ]tetradeca-2,4,6-trien-6,9-diyl diacetate (31 mg).

後処理

  1. filtrationThe reaction mixture was filtered through cellulose powder
  2. customthe filtrate was evaporated in vacuo
  3. additionwas developed with a mixture of chloroform and methanol (10:1

出典と根拠

ORDレコード
ord-46da3ac7ab084b42904894077c67d075
出典データセット
uspto-grants-1988_05
特許番号
US04743555

反応ノート

読み込み中…