反応 #94722

反応方程式

2-amino-4,5,6-trimethylpyrimidine

methylene chloride

methyl 2-(isocyanatosulfonyl)benzoate

→

Methyl 2-{[(4,5,6-trimethylpyrimidin-2-yl)aminocarbonyl]-aminosulfonyl}benzoate

溶媒

Butyl chloride

反応条件

後処理

1. 1
   workup.STIRRINGwith constant stirring
2. 2
   ろ過the insoluble product filtered
3. 3
   洗浄washed immediately with butyl chloride
4. 4
   その他dried

実験手順

To a mixture of 1.0 gram (0.0073 mole) of 2-amino-4,5,6-trimethylpyrimidine and 5.0 ml of dried methylene chloride stirring magnetically in a 50 ml RB single neck flask, 2.1 grams of methyl 2-(isocyanatosulfonyl)benzoate was added at room temperature and the mixture stirred at room temperature for 24 hours. Butyl chloride (4 ml) was added with constant stirring and the insoluble product filtered, washed immediately with butyl chloride and dried. (Yield 1.3 grams, m.p. 152°-161°). IR (Nujol): 5.60, 5.75 (C=O), 11.25 11.90 microns; NMR (TFA-d): δ2.30 (s,3H,CH3), 2.65 (s, 6H, 2CH3), 4.00 (s, 3H, CO2CH3), 7.60-8.60 (m, ArH).

出典