反応 #1583877

反応方程式

methanol

2,2-diphenylacetic acid

oxalyl chloride

→

methyl 2,2-diphenylacetate

収率 98.7%

溶媒

DMF

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   その他was conducted at 25° C
2. 2
   その他After the completion of reaction
3. 3
   その他the mixture was evaporated under reduced pressure
4. 4
   その他to remove oxalyl chloride
5. 5
   温度under cooling in an ice bath respectively
6. 6
   その他was conducted at 25° C
7. 7
   その他After the completion of reaction
8. 8
   洗浄the reaction solution was washed with a saturated aqueous NaCl solution
9. 9
   乾燥The organic phase was dried over sodium sulfate
10. 10
    ろ過filtered by suction
11. 11
    その他The filtrate was evaporated to dryness

実験手順

To a 500 mL three-opening flask were added 2,2-diphenylacetic acid (20 g, 94 mmol) and 200 mL dichloromethane. After stirring, 1 mL DMF was added. To the mixture was slowly added oxalyl chloride (13.16 g, 104 mmol) dropwisely in an ice bath. The reaction was conducted at 25° C. After the completion of reaction, the mixture was evaporated under reduced pressure to remove oxalyl chloride. To the reaction flask were slowly added dichloromethane (100 mL) and anhydrous methanol (3.61 g, 113 mmol) dropwisely under cooling in an ice bath respectively. The reaction was conducted at 25° C. After the completion of reaction, the reaction solution was washed with a saturated aqueous NaCl solution. The organic phase was dried over sodium sulfate, and filtered by suction. The filtrate was evaporated to dryness to produce methyl 2,2-diphenylacetate (21 g) in a yield of 98.7%.

出典