反応 #619083

反応方程式

Dicyclohexylamine

aminothiazole

carbonyldiimidazole

→

title product

1,1-Dicyclohexyl-3-thiazol 2 yl urea

溶媒

ethyl acetate

dichloromethane

反応条件

後処理

1. 1
   workup.STIRRINGthe reaction stirred overnight at room temperature
2. 2
   洗浄washed successively with 10% sodiumhydrogensulphate (3 mL), water (3 mL)
3. 3
   乾燥dried over magnesium sulphate
4. 4
   濃縮concentrated in vacuo
5. 5
   その他the residue purified by HPLC (Gilson 1, X-terra column; 0-100% CH3CN/H2O/0, 1% TFA; 15 min; flow 50 ml/min)

実験手順

To a solution of aminothiazole (50 mg, 0.5 mmol) in dichloromethane was added carbonyldiimidazole (81 mg, 0.5 mmol) and the solution stirred 2 h at room temperature. Dicyclohexylamine (1 eq) was then added and the reaction stirred overnight at room temperature. The reaction mixture is then diluted with ethyl acetate (8 mL), washed successively with 10% sodiumhydrogensulphate (3 mL), water (3 mL), dried over magnesium sulphate, concentrated in vacuo, and the residue purified by HPLC (Gilson 1, X-terra column; 0-100% CH3CN/H2O/0, 1% TFA; 15 min; flow 50 ml/min) to give the title product (52 mg).

出典