反应 #607488

ord-adb298f8946e41fbbb0ca163a4ad0259

反应方程式

CC1(C)CNC(C(=O)O)C1
4,4-dimethylpyrrolidine-2-carboxylic acid
O=C(Cl)CCN1C(=O)c2ccccc2C1=O
137h
O=C(Cl)CCN1C(=O)c2ccccc2C1=O
3-(1,3-dioxoisoindolin-2-yl)propanoyl chloride
CC1(C)CC(C(=O)O)N(C(=O)CCN2C(=O)c3ccccc3C2=O)C1
1-(3-(1,3-dioxoisoindolin-2-yl)propanoyl)-4,4-dimethylpyrrolidine-2-carboxylic acid

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Upon reaction completion
  2. 2
    洗涤the mixture was washed with brine (50 mL×3)
  3. 3
    干燥dried over anhydrous sodium sulfate
  4. 4
    过滤filtered
  5. 5
    浓缩concentrated under reduced pressure

实验过程

To a solution of 4,4-dimethylpyrrolidine-2-carboxylic acid 137f (13.0 g, 72.5 mmol) in DMF (250 mL) was added 137h (17.0 g, 72.5 mmol) and TEA (14.5 g, 145 mmol). See FIG. 2. The mixture was stirred at RT (room temperature) for 16 h (sixteen hours). Upon reaction completion, the mixture was washed with brine (50 mL×3), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to give crude 1-(3-(1,3-dioxoisoindolin-2-yl)propanoyl)-4,4-dimethylpyrrolidine-2-carboxylic acid 137i, which was used directly without purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09326985B2uspto-grants-2016_05