반응 #9787

ord-91be913968d14eb2aa60244378ae719c

반응 방정식

CCOC(=O)COc1ccc(C(C)(C)C(=O)c2sc(-c3ccc(C(F)(F)F)cc3)cc2C)cc1C
ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate
CCOC(=O)COc1ccc(C(C)(C)C(=O)c2sc(-c3ccc(C(F)(F)F)cc3)cc2C)cc1C
intermediate 106
CCOC(=O)COc1ccc(C(C)(C)C(=O)c2sc(-c3ccc(C(F)(F)F)cc3)cc2C)cc1C
ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate
O=C(O)C(F)(F)F
trifluoroacetic acid
CC[SiH](CC)CC
triethylsilane
CCOC(=O)COc1ccc(C(C)(C)Cc2sc(-c3ccc(C(F)(F)F)cc3)cc2C)cc1C
title compound
CCOC(=O)COc1ccc(C(C)(C)Cc2sc(-c3ccc(C(F)(F)F)cc3)cc2C)cc1C
ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}ethyl)-2-methylphenoxy]acetate

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The vial was then sealed
  2. 2
    온도to cool to room
  3. 3
    농축concentrated in vacuo
  4. 4
    기타Purification by flash column chromatography
  5. 5
    세척eluting cyclohexane-1% EtOAc/cyclohexane

실험 절차

To a reactivial containing ethyl[4-(1,1-dimethyl-2-{3-methyl-5-[4-(trifluoromethyl)phenyl]thien-2-yl}-2-oxoethyl)-2-methylphenoxy]acetate (intermediate 106, 36 mg) was added trifluoroacetic acid (0.22 ml) and triethylsilane (0.11 ml). The vial was then sealed and heated at 50° C. for 18 hours. The reaction was then allowed to cool to room and concentrated in vacuo. Purification by flash column chromatography eluting cyclohexane-1% EtOAc/cyclohexane yielded the title compound as a colourless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091237B2uspto-grants-2006_08