Iodine → HCID 544889、化合物

HRID 1719520ノート

反応式

HRID 1719520 の反応式
CO.II.OC1C=CC=CC=1CC1(NCC2C=CC=CC=2)CCCCC1.[C:27]([C:35]1[CH2:40][CH2:39][CH2:38][CH2:37][C:36]=1[NH:41]CC1C=CC=CC=1)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>[Pd].C(Cl)Cl>[OH:34][CH:27]([C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1)[CH:35]1[CH2:40][CH2:39][CH2:38][CH2:37][CH:36]1[NH2:41]

参加物

7

反応物 4

HCID 807IodineHCID 887MethanolHCID 319570[2-(Benzylamino)cyclohex-1-en-1-yl](phenyl)methanone2 回HCID 20211919HCID 20211919、化合物

生成物 1

HCID 544889HCID 544889、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 6344Dichloromethane溶媒

実験手順

A 17.9 kg lot of N-[2-(benzoyl)-cyclohexen-1-yl]benzylamine in ethanol solution from Step B above, was hydrogenated at 100 psig over 10% palladium on carbon (1800 g) in a 20 or 30 gallon autoclave. The reduction required 18 days for completion. The hydrogenation reaction was monitored periodically by thin layer chromatography (tlc) analyses using alumina GF plates (Analtech) and 5% methanol in methylene chloride. The plates were visualized with iodine. The reduction proceeds through the intermediate N-[[2(hydroxy)phenylmethyl]cyclohexyl]benzylamine which was evident by the tlc methods.

後処理

  1. custom18 days
  2. customThe hydrogenation reaction

出典と根拠

ORDレコード
ord-59f553b4b7984401bad747bb7753f656
出典データセット
uspto-grants-1985_09
特許番号
US04540690

反応ノート

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