Hydrochloric Acid → HCID 22857049、化合物

HRID 2211410ノート

反応式

HRID 2211410 の反応式
[C:1]1([C:7]2([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[C@@H:15]3[C@@H:11]([CH2:12][N:13](C(OC(C)(C)C)=O)[CH2:14]3)[C@@:10]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])(O)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:38]>C(O)(=O)C>[ClH:38].[C:32]1([C:7]2([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8][CH:9]=[C:10]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])[C@H:11]3[C@@H:15]2[CH2:14][NH:13][CH2:12]3)[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 22857048HCID 22857048、化合物

生成物 1

HCID 22857049HCID 22857049、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 8.56 g of (3aS,4S,7aS)-7,7-diphenyl-4-(2-methoxyphenyl)-2-tert-butoxycarbonyl-perhydroisoindol-4-ol in 53 cm3 of acetic acid and 30 cm3 of 12N hydrochloric acid is heated at 95° C. for 45 minutes, and then cooled to room temperature and concentrated to dryness under reduced pressure (2.7 kPa). The residue is recrystallised from 20 cm3 of acetonitrile. 5.2 g of (3aS,7aR)-4,4-diphenyl-7-(2-methoxyphenyl)-2,3,3a, 4,5,7a-hexahydroisoindole hydrochloride are obtained in the form of white crystals which melt at a temperature above 300° C., and the product is used in the crude state in the subsequent syntheses.

後処理

  1. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  2. customThe residue is recrystallised from 20 cm3 of acetonitrile

出典と根拠

ORDレコード
ord-2f900bf2c8484294ac0ea55502ed1e00
出典データセット
uspto-grants-1995_10
特許番号
US05463077

反応ノート

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