1-[[[4-(4-Propylpiperazin-1-yl)phenyl]carbonyl]amino]cyclohexanecarboxylic acid hydrochloride → 2-[4-(4-Propylpiperazin-1-yl)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-en-4-one hydrochloride

HRID 1851823노트

반응식

HRID 1851823 반응식
[ClH:1].[CH2:2]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([NH:19][C:20]3([C:26]([OH:28])=[O:27])[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]3)=O)=[CH:13][CH:12]=2)[CH2:7][CH2:6]1)[CH2:3][CH3:4]>C(OC(=O)C)(=O)C>[ClH:1].[CH2:2]([N:5]1[CH2:6][CH2:7][N:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]3[O:28][C:26](=[O:27])[C:20]4([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25]4)[N:19]=3)=[CH:13][CH:12]=2)[CH2:9][CH2:10]1)[CH2:3][CH3:4]

참가 물질

3

반응물 1

HCID 671808091-[[[4-(4-Propylpiperazin-1-yl)phenyl]carbonyl]amino]cyclohexanecarboxylic acid hydrochloride

생성물 1

HCID 671807462-[4-(4-Propylpiperazin-1-yl)phenyl]-3-oxa-1-azaspiro[4.5]dec-1-en-4-one hydrochloride수율 83%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

반응 조건

온도
100 °C

실험 절차

After a suspension of 631 mg (1.54 mmol) of 1-[[[4-(4-propylpiperazin-1-yl)phenyl]carbonyl]amino]cyclohexanecarboxylic acid hydrochloride in 18 ml of acetic anhydride was stirred at 100° C. for 1 hour, the reaction solution was concentrated under reduced pressure. The operation for adding toluene to the obtained residue and distilling off it under reduced pressure was carried out three times, and acetic anhydride was removed by azeotropic distillation to obtain 500 mg (83%) of the title compound.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. additionThe operation for adding toluene to the obtained residue
  3. distillationdistilling off it under reduced pressure
  4. customwas removed by azeotropic distillation

출처 및 근거

ORD 기록
ord-e4aa52b5772a4913874be8192cdfb576
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957205B2

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