Citric Acid → 2-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid citrate

HRID 582778

반응식

HRID 582778 반응식
[C:1]([OH:13])(=[O:12])[CH2:2][C:3]([CH2:8][C:9]([OH:11])=[O:10])([C:5]([OH:7])=[O:6])[OH:4].[CH3:14][O:15][C:16]1[CH:21]=[CH:20][CH:19]=[C:18]([O:22][CH3:23])[C:17]=1[C:24]1[N:28]([C:29]2[CH:34]=[CH:33][C:32]([C:35](=[O:44])[N:36]([CH3:43])[CH2:37][CH2:38][CH2:39][N:40]([CH3:42])[CH3:41])=[CH:31][C:30]=2[CH:45]([CH3:47])[CH3:46])[N:27]=[C:26]([C:48]([NH:50][C:51]2([C:61]([OH:63])=[O:62])[CH:58]3[CH2:59][CH:54]4[CH2:55][CH:56]([CH2:60][CH:52]2[CH2:53]4)[CH2:57]3)=[O:49])[CH:25]=1>CCO.C(Cl)Cl>[C:1]([OH:13])(=[O:12])[CH2:2][C:3]([CH2:8][C:9]([OH:11])=[O:10])([C:5]([OH:7])=[O:6])[OH:4].[CH3:23][O:22][C:18]1[CH:19]=[CH:20][CH:21]=[C:16]([O:15][CH3:14])[C:17]=1[C:24]1[N:28]([C:29]2[CH:34]=[CH:33][C:32]([C:35](=[O:44])[N:36]([CH3:43])[CH2:37][CH2:38][CH2:39][N:40]([CH3:41])[CH3:42])=[CH:31][C:30]=2[CH:45]([CH3:47])[CH3:46])[N:27]=[C:26]([C:48]([NH:50][C:51]2([C:61]([OH:63])=[O:62])[CH:52]3[CH2:53][CH:54]4[CH2:55][CH:56]([CH2:57][CH:58]2[CH2:59]4)[CH2:60]3)=[O:49])[CH:25]=1

참가 물질

5

반응물 2

HCID 311Citric AcidHCID 5311451SR142948A

생성물 1

HCID 702406642-[5-(2,6-Dimethoxyphenyl)-1-[4-[N-methyl-N-(3-dimethylaminopropyl)carbamoyl]-2-isopropylphenyl]-3-pyrazolylcarbonylamino]-2-adamantanecarboxylic acid citrate수율 67.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6344Dichloromethane용매

실험 절차

0.084 g of citric acid is added at RT to a solution of 0.3 g of the compound obtained in EXAMPLE 1' in 5 ml of EtOH and 3 ml of DCM, and the mixture is left stirring for 2 hours at RT. It is concentrated under vacuum and the residue is recrystallized in 2-propanol. 0.26 g of the expected product is obtained, m.p.=168° C.

후처리

  1. concentrationIt is concentrated under vacuum
  2. customthe residue is recrystallized in 2-propanol

출처 및 근거

ORD 기록
ord-d90b201a01c74d358cc671790aca019c
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05925661

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