반응 #61541

ord-a547fe0344f84561a66ac7a3a0247452

반응 방정식

Cl
HCl
O=C(O)c1cc(CO)nn1Cc1cc(-c2ccc(Cl)s2)on1
2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-hydroxymethyl-2H-pyrazole-3-carboxylic acid
COCCBr
1-Bromo-2-methoxy-ethane
COCCOCc1cc(C(=O)O)n(Cc2cc(-c3ccc(Cl)s3)on2)n1
2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-(2-methoxy-ethoxymethyl)-2H-pyrazole-3-carboxylic acid

용매

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered through a chem elut® cartridge by elution with ethyl acetate
  2. 2
    농축After concentration the crude product
  3. 3
    기타was directly subjected to the next reaction step

실험 절차

To a solution of 500 mg of 2-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-5-hydroxymethyl-2H-pyrazole-3-carboxylic acid in 5 ml DMF 480 mg Cs2CO3 and 204 mg 1-Bromo-2-methoxy-ethane were added and the mixture was heated to 80° C. for 5 h. Then the mixture was acidified to pH 4 with aqueous HCl and filtered through a chem elut® cartridge by elution with ethyl acetate. After concentration the crude product was directly subjected to the next reaction step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07429581B2uspto-grants-2008_09