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

HRID 2291551

반응식

HRID 2291551 반응식
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

참가 물질

3

반응물 1

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

생성물 1

HCID 131083KB-5492 free base수율 76%

시약·촉매·용매 1

HCID 11430Potassium Carbonate용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3fefa20d7a8d4f0bbf393a8f8e39eaa1
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04797400

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