Hydrochloric Acid → Piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride

HRID 550810노트

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HRID 550810 반응식
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][N:12]([C:15](=[O:28])[NH:16][C:17]2[S:18][C:19]3[N:20]=[CH:21][N:22]=[C:23]([O:26][CH3:27])[C:24]=3[N:25]=2)[CH2:11][CH2:10]1)=O)(C)(C)C>C(Cl)Cl>[ClH:1].[CH3:27][O:26][C:23]1[C:24]2[N:25]=[C:17]([NH:16][C:15]([N:12]3[CH2:11][CH2:10][NH:9][CH2:14][CH2:13]3)=[O:28])[S:18][C:19]=2[N:20]=[CH:21][N:22]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 590119304-(7-Methoxy-thiazolo[5,4-d]pyrimidin-2-ylcarbamoyl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 86616506Piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

Hydrogen chloride gas was bubbled through a solution of 4-(7-methoxy-thiazolo[5,4-d]pyrimidin-2-ylcarbamoyl)-piperazine-1-carboxylic acid tert-butyl ester (5.20 g, 13 mmol) in methylene chloride (70 mL) for 10 min at 0° C. A white precipitate formed. The resulting slurry was stirred at 25° C. for 2 h. At this time, the mixture was concentrated in vacuo and dried under high vacuum to afford piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide hydrochloride (4.61 g) as a white solid; LRMS for C11H14N6O2S (M+H)+ at m/z=295. This solid was used in the next step without further purification.

후처리

  1. customA white precipitate formed
  2. concentrationAt this time, the mixture was concentrated in vacuo
  3. customdried under high vacuum

출처 및 근거

ORD 기록
ord-ff6a7e27a8fb403d85a3024830d7eaee
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947692B2

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