تفاعل #1583877

معادلة التفاعل

methanol

2,2-diphenylacetic acid

oxalyl chloride

→

methyl 2,2-diphenylacetate

المردود 98.7%

المذيبات

DMF

dichloromethane

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىwas conducted at 25° C
2. 2
   أخرىAfter the completion of reaction
3. 3
   أخرىthe mixture was evaporated under reduced pressure
4. 4
   أخرىto remove oxalyl chloride
5. 5
   درجة الحرارةunder cooling in an ice bath respectively
6. 6
   أخرىwas conducted at 25° C
7. 7
   أخرىAfter the completion of reaction
8. 8
   غسيلthe reaction solution was washed with a saturated aqueous NaCl solution
9. 9
   تجفيفThe organic phase was dried over sodium sulfate
10. 10
    ترشيحfiltered by suction
11. 11
    أخرىThe filtrate was evaporated to dryness

الإجراء التجريبي

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%.

المصدر