Hydrochloric Acid → 4-(2,2-Dimethylpropionyloxy)pyrazolidine-1-carboxylic acid 1-benzyl ester

HRID 7656

反応式

HRID 7656 の反応式
C(OC([N:8]1[CH2:12][CH:11]([O:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[CH2:10][N:9]1[C:20]([O:22][CH2:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[O:21])=O)(C)(C)C.S(Cl)(Cl)=O.Cl>CO>[CH2:23]([O:22][C:20]([N:9]1[CH2:10][CH:11]([O:13][C:14](=[O:19])[C:15]([CH3:17])([CH3:16])[CH3:18])[CH2:12][NH:8]1)=[O:21])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 207247514-(2,2-Dimethylpropionyloxy)pyrazolidine-1,2-dicarboxylic acid 1-benzyl ester 2-tert-butyl ester

生成物 1

HCID 207247484-(2,2-Dimethylpropionyloxy)pyrazolidine-1-carboxylic acid 1-benzyl ester収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

4-(2,2-Dimethylpropionyloxy)pyrazolidine-1,2-dicarboxylic acid 1-benzyl ester 2-tert-butyl ester, 29, (1.76 g, 4.33 mmol) is dissolved in methanol (40 mL) and the solution cooled to 0° C. Thionyl chloride (3.16 mL, 43.3 mmol) is added dropwise and the reaction allowed to warm to room temperature and continue stirring 12 hours. The reaction solution is concentrated in vacuo to give afford 1.45 g (98% yield) of the desired product as the HCl salt as an off-white solid.

後処理

  1. temperatureto warm to room temperature
  2. concentrationThe reaction solution is concentrated in vacuo
  3. customto give

出典と根拠

ORDレコード
ord-95bc99090f3e498c8ea0e5f42c1b5fc5
出典データセット
uspto-grants-2006_08
特許番号
US07087615B2

関連ノート

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