반응 #619083

ord-dcf5ebbe7d3e40ecb5e3a5bbd7e135a5

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE045183E1uspto-grants-2014_10