1-[(4-Methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride → KB-5492 free base

HRID 2291551

反応式

HRID 2291551 の反応式
Cl.Cl.[CH3:3][O:4][C:5]1[CH:33]=[CH:32][C:8]([O:9][C:10]([CH2:12][N:13]2[CH2:18][CH2:17][N:16]([CH2:19][C:20]3[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[C:22]([O:30][CH3:31])[CH:21]=3)[CH2:15][CH2:14]2)=[O:11])=[CH:7][CH:6]=1>C(=O)([O-])[O-].[K+].[K+]>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([O:9][C:10]([CH2:12][N:13]2[CH2:14][CH2:15][N:16]([CH2:19][C:20]3[CH:25]=[C:24]([O:26][CH3:27])[C:23]([O:28][CH3:29])=[C:22]([O:30][CH3:31])[CH:21]=3)[CH2:17][CH2:18]2)=[O:11])=[CH:32][CH:33]=1

参加物

3

反応物 1

HCID 141001161-[(4-Methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride

生成物 1

HCID 131083KB-5492 free base収率 76%

試薬・触媒・溶媒 1

HCID 11430Potassium Carbonate溶媒

実験手順

The 1-[(4-methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (8.0 g) obtained above is added to a 5% aqueous potassium carbonate solution (100 ml), and the produced oily substance is extracted with chloroform (150 ml). The chloroform layer is dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. The residue is recrystallized from a mixture of ethyl acetate and n-hexane to give 1-[(4-methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine (5.2 g).

後処理

  1. extractionthe produced oily substance is extracted with chloroform (150 ml)
  2. dry with materialThe chloroform layer is dried over anhydrous magnesium sulfate
  3. distillationthe solvent is distilled off under reduced pressure
  4. customThe residue is recrystallized from a mixture of ethyl acetate and n-hexane

出典と根拠

ORDレコード
ord-3fefa20d7a8d4f0bbf393a8f8e39eaa1
出典データセット
uspto-grants-1989_01
特許番号
US04797400

関連ノート

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