تفاعل #70566

معادلة التفاعل

1-(2-phenylpyrimidin-5-yl)ethanone

tetrabutylammonium tribromide

→

title intermediate

المردود 79.4%

2-bromo-1-(2-phenylpyrimidin-5-yl)ethanone

المردود 79.4%

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction mixture was sealed with a screw top
2. 2
   درجة الحرارةto cool to room temperature over a weekend
3. 3
   أخرىThe pale yellow precipitate formed
4. 4
   أخرىwas collected on
5. 5
   ترشيحa filter
6. 6
   غسيلwashed with 1:1 dichloromethane-hexane

الإجراء التجريبي

To a solution consisting of 1-(2-phenylpyrimidin-5-yl)ethanone (Step A, 700 mg, 3.5 mmol) in dichloromethane (25 mL) was added tetrabutylammonium tribromide (1.87 g, 3.90 mmol). The reaction mixture was sealed with a screw top and warmed at 40° C. for 5 hours and allowed to cool to room temperature over a weekend. The pale yellow precipitate formed was collected on a filter and washed with 1:1 dichloromethane-hexane to afford the title intermediate (770 mg, 79%); Rf 0.31 with 9:1 v/v hexanes-ethyl acetate; MS (ESI+) m/z 279, 277 (M+1, Br isotopes).

المصدر