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

HRID 550810ノート

反応式

HRID 550810 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-ff6a7e27a8fb403d85a3024830d7eaee
出典データセット
uspto-grants-2011_05
特許番号
US07947692B2

反応ノート

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