反応 #57060

反応方程式

HCl

n-BuI

LDA

cyclobutane carboxylic acid

→

title compound

1-butylcyclobutanecarboxylic acid

溶媒

THF heptane ethylbenzene

THF

反応条件

後処理

1. 1
   workup.ADDITIONAfter addition
2. 2
   その他the cold bath was removed
3. 3
   workup.STIRRINGThe mixture was stirred over night
4. 4
   抽出the mixture was extracted with ethyl acetate
5. 5
   洗浄The combined organic phase was washed with water and brine

実験手順

To a solution of LDA (30 mL, 2.0M, 60 mmol) in THF/heptane/ethylbenzene and anhydrous THF (30 mL) at 0° C. was added cyclobutane carboxylic acid (3.0 g, 30 mmol) dropwise. After addition was complete, the cold bath was removed, the reaction mixture was stirred at room temperature for 2 hr. Neat n-BuI (3.41 mL, 30 mmol) was added dropwise at room temperature. The mixture was stirred over night. To the mixture was added 2N HCl and the mixture was extracted with ethyl acetate. The combined organic phase was washed with water and brine to afford the title compound as a light yellow oil (quantitative), which was used in the next step without purification.

出典