反応 #607488

ord-adb298f8946e41fbbb0ca163a4ad0259

反応方程式

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

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Upon reaction completion
  2. 2
    洗浄the mixture was washed with brine (50 mL×3)
  3. 3
    乾燥dried over anhydrous sodium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure

実験手順

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.

出典

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