反应 #619083

ord-dcf5ebbe7d3e40ecb5e3a5bbd7e135a5

反应方程式

C1CCC(NC2CCCCC2)CC1
Dicyclohexylamine
Nc1nccs1
aminothiazole
O=C(n1ccnc1)n1ccnc1
carbonyldiimidazole
O=C(Nc1nccs1)N(C1CCCCC1)C1CCCCC1
title product
O=C(Nc1nccs1)N(C1CCCCC1)C1CCCCC1
1,1-Dicyclohexyl-3-thiazol 2 yl urea

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE045183E1uspto-grants-2014_10