(3aR*,10aS*)-9-[4-(benzyloxycarbonylamino)benzyl]-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one → (3aR*,10aS*)-9-(4-Aminobenzyl)-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e]-[1,4]diazepin-10(1H)-one hydrobromide

HRID 361570ノート

反応式

HRID 361570 の反応式
C(OC([NH:11][C:12]1[CH:47]=[CH:46][C:15]([CH2:16][N:17]2[C:23](=[O:24])[C@H:22]3[CH2:25][CH2:26][CH2:27][C@H:21]3[N:20]([C:28](=[O:41])[CH2:29][N:30]3[C:34](=[O:35])[C:33]4=[CH:36][CH:37]=[CH:38][CH:39]=[C:32]4[C:31]3=[O:40])[C:19]3[CH:42]=[CH:43][CH:44]=[CH:45][C:18]2=3)=[CH:14][CH:13]=1)=O)C1C=CC=CC=1.[BrH:48].C(O)(=O)C>C(Cl)(Cl)Cl>[BrH:48].[NH2:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:16][N:17]2[C:23](=[O:24])[C@H:22]3[CH2:25][CH2:26][CH2:27][C@H:21]3[N:20]([C:28](=[O:41])[CH2:29][N:30]3[C:31](=[O:40])[C:32]4=[CH:39][CH:38]=[CH:37][CH:36]=[C:33]4[C:34]3=[O:35])[C:19]3[CH:42]=[CH:43][CH:44]=[CH:45][C:18]2=3)=[CH:46][CH:47]=1

参加物

4

反応物 2

HCID 15385743(3aR*,10aS*)-9-[4-(benzyloxycarbonylamino)benzyl]-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-oneHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

生成物 1

HCID 67767990(3aR*,10aS*)-9-(4-Aminobenzyl)-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e]-[1,4]diazepin-10(1H)-one hydrobromide収率 92%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of (3aR*,10aS*)-9-[4-(benzyloxycarbonylamino)benzyl]-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (366 mg, 0.58 mmol) in chloroform (3 mL) was added 25% hydrogen bromide/acetic acid (1 mL) and the mixture was stirred at room temperature for 75 minutes. This reaction mixture was concentrated under reduced pressure and the residue was crystallized from ethanoldiethyl ether to provide 309 mg (yield 92%) of the title compound. m.p. 222°-224° C.

後処理

  1. concentrationThis reaction mixture was concentrated under reduced pressure
  2. customthe residue was crystallized from ethanoldiethyl ether

出典と根拠

ORDレコード
ord-dc7cda3d08c24748a8e184060a5055c6
出典データセット
uspto-grants-1999_02
特許番号
US05866567

反応ノート

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