Hydrochloric Acid → 4'-[4-[4-(cis-2,6-Dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1'-biphenyl-4-carboxylic acid

HRID 1816756노트

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C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([N:17]3[CH2:22][CH2:21][N:20]([C:23]4[CH:28]=[CH:27][C:26]([N:29]5[CH2:34][C@H:33]([CH3:35])[O:32][C@H:31]([CH3:36])[CH2:30]5)=[CH:25][CH:24]=4)[CH2:19][CH2:18]3)=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].CO.Cl>O.O1CCCC1>[CH3:35][C@H:33]1[O:32][C@@H:31]([CH3:36])[CH2:30][N:29]([C:26]2[CH:25]=[CH:24][C:23]([N:20]3[CH2:19][CH2:18][N:17]([C:14]4[CH:15]=[CH:16][C:11]([C:8]5[CH:9]=[CH:10][C:5]([C:3]([OH:4])=[O:2])=[CH:6][CH:7]=5)=[CH:12][CH:13]=4)[CH2:22][CH2:21]3)=[CH:28][CH:27]=2)[CH2:34]1

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실험 절차

A mixture of 4′-[4-[4-(cis-2,6-dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1′-biphenyl-4-carboxylic acid methyl ester (3.70 g) and 1.0 mol/l sodium hydroxide solution (30 ml) in a mixed solvent of methanol (75 ml) and tetrahydrofuran (185 ml) was refluxed for 15.5 hours. After cooling to ambient temperature, the reaction mixture was poured into cold water, and the mixture was adjusted to pH 2 with 1.0 mol/l hydrochloric acid. The resulting precipitates were filtered, washed with water and diisopropyl ether and dried to give 4′-[4-[4-(cis-2,6-dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1′-biphenyl-4-carboxylic acid (3.68 g).

후처리

temperaturewas refluxed for 15.5 hours
customThe resulting precipitates
filtrationwere filtered
washwashed with water and diisopropyl ether
customdried

출처 및 근거

ORD 기록: ord-2ca87cb8a54e4f1c9b51de002c1fd3ba
출처 데이터셋: uspto-grants-2005_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06884868B1

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