反応 #2271295

反応方程式

7-Bromo-4-chloro-2,2-diphenyl-benzo[1,3]dioxole-5-carboxylic acid methyl ester

Lithium hydroxide hydrate

methanol

→

7-bromo-4-chloro-2,2-diphenyl-benzo[1,3]dioxole-5-carboxylic acid

溶媒

THF

water

反応条件

後処理

1. 1
   温度is heated
2. 2
   温度to reflux for 5 hours
3. 3
   温度After cooling the organic solvents
4. 4
   その他are evaporated
5. 5
   workup.ADDITIONthe reaction is diluted with water
6. 6
   抽出extracted with ethyl acetate
7. 7
   洗浄The combined organic layers are washed with brine
8. 8
   ろ過filtered
9. 9
   その他The solvent is evaporated in vacuo
10. 10
    その他The product precipitates as a white solid (350 mg, 70%), which
11. 11
    ろ過is filtered
12. 12
    その他dried

実験手順

7-Bromo-4-chloro-2,2-diphenyl-benzo[1,3]dioxole-5-carboxylic acid methyl ester (520 mg, 1.16 mmol) is dissolved in THF (6 ml). Lithium hydroxide hydrate (190 mg, 4.64 mmol) in water (6 ml) is added. After addition of methanol (2 ml) the reaction is heated to reflux for 5 hours. After cooling the organic solvents are evaporated and the reaction is diluted with water, acidified with 1N aqueous HCl solution and extracted with ethyl acetate. The combined organic layers are washed with brine, dired over sodium sulfate and filtered. The solvent is evaporated in vacuo. The residue is stirred with n-hexane. The product precipitates as a white solid (350 mg, 70%), which is filtered and dried.

出典