Sodium Bicarbonate → KB-5492 free base

HRID 2291550

반응식

HRID 2291550 반응식
Cl.Cl.[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:15]=[C:16]([O:20][CH3:21])[C:17]=1[O:18][CH3:19])[CH2:8][N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.Cl[CH2:23][C:24]([O:26][C:27]1[CH:32]=[CH:31][C:30]([O:33][CH3:34])=[CH:29][CH:28]=1)=[O:25].C(=O)([O-])O.[Na+]>C(#N)C>[CH3:34][O:33][C:30]1[CH:31]=[CH:32][C:27]([O:26][C:24]([CH2:23][N:12]2[CH2:13][CH2:14][N:9]([CH2:8][C:7]3[CH:6]=[C:5]([O:4][CH3:3])[C:17]([O:18][CH3:19])=[C:16]([O:20][CH3:21])[CH:15]=3)[CH2:10][CH2:11]2)=[O:25])=[CH:28][CH:29]=1

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 5324604-Methoxyphenyl chloroacetateHCID 128285011-[(3,4,5-Trimethoxyphenyl)methyl]piperazine;dihydrochloride

생성물 1

HCID 131083KB-5492 free base

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

A mixture of 1-(3,4,5-trimethoxybenzyl)piperazine dihydrochloride (prepared by the method disclosed in Belgian Pat. No. 560,330) (50 g), 4-methoxyphenyl chloroacetate (prepared by the method disclosed in U.S. Pat. No. 3,657,318) (33 g), sodium hydrogen carbonate (49 g) and acetonitrile (700 ml) is stirred at 60° C. for 3 hours. The reaction mixture is filtered, and the filtrate is concentrated under reduced pressure to give crude 1-[(4-methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine (free base) (60 g) as an oily substance. This crude free base (60 g) is dissolved in a mixture of water (200 ml) and acetonitrile (50 ml) and thereto is added fumaric acid of about 2 moles (41 g) to 1 mole of the free base, and the mixture is heated. After the reaction mixture is allowed to cool at room temperature, the precipitated crystals are separated by filtration and recrystallized from a mixture of water and acetonitrile to give 1-[(4-methoxyphenoxy)carbonylmethyl]-4-(3,4,5-trimethoxybenzyl)piperazine difumarate monohydrate (73.5 g) as colorless crystals.

후처리

  1. customprepared by the method
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-144f365eac6449b9a22af2d25fd6e072
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04797400

연결된 노트

불러오는 중…