(RS)-N,N-dimethyl-{2-[4-(alpha-phenyl-p-chloro-benzyl)piperazin-1-yl]ethoxy}-acetamide dihydrochloride → Cetirizine Hydrochloride

HRID 1072262

반응식

HRID 1072262 반응식
Cl.Cl.CN(C)[C:5](=[O:30])[CH2:6][O:7][CH2:8][CH2:9][N:10]1[CH2:15][CH2:14][N:13]([CH:16]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)[CH2:12][CH2:11]1.C(O)(=O)/C=C/C(O)=[O:36].CN(C)C(=O)COCCN1CCN(C(C2C=CC=CC=2)C2C=CC([Cl:60])=CC=2)CC1>>[ClH:23].[ClH:60].[C:24]1([CH:16]([N:13]2[CH2:14][CH2:15][N:10]([CH2:9][CH2:8][O:7][CH2:6][C:5]([OH:30])=[O:36])[CH2:11][CH2:12]2)[C:17]2[CH:18]=[CH:19][C:20]([Cl:23])=[CH:21][CH:22]=2)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

3

반응물 2

HCID 22391908(RS)-N,N-dimethyl-{2-[4-(alpha-phenyl-p-chloro-benzyl)piperazin-1-yl]ethoxy}-acetamide dihydrochlorideHCID 22391911(RS)-N,N-dimethyl-{2-[4-(alpha-phenyl-p-chloro-benzyl)piperazin-1-yl]ethoxy}-acetamide fumarate

생성물 1

HCID 55182Cetirizine Hydrochloride수율 77.8%

실험 절차

The procedure described in Example 13 is followed with the difference that, instead of the (RS)-N,N-dimethyl-{2-[4-(α-phenyl-p-chloro-benzyl)piperazin-1-yl]ethoxy}-acetamide dihydrochloride, 106.4 g (0.2 moles) of (RS)-N,N-dimethyl-{2-[4-(α-phenyl-p-chloro-benzyl)piperazin-1-yl]ethoxy}-acetamide fumarate is used, and, after adjusting the pH of the reaction mixture to 3.8, the precipitated fumaric acid is filtered to facilitate the extraction with dichloromethane. Thus, 71.8 g (77.8%) of the title compound are obtained, m.p.: 225-228° C. The purity of the product corresponds to the quality requirements given in Eur. Pharm., 3, 1997, 1084.

후처리

  1. filtrationthe precipitated fumaric acid is filtered
  2. extractionthe extraction with dichloromethane

출처 및 근거

ORD 기록
ord-39b56c52380e47fe8dc73857565a99ab
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06908999B2

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