تفاعل #1435741

ord-d21304687d344c469bf0781504bb0076

معادلة التفاعل

CI
iodomethane
CN1CCN(c2cc(I)c(NC(=O)C(C)(C)c3cc(C(F)(F)F)cc(C(F)(F)F)c3)cn2)CC1
2-(3,5-bis-trifluoromethyl-phenyl)-N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-isobutyramide
C[Si](C)(C)[N-][Si](C)(C)C.[K+]
potassium bis(trimethylsilyl)amide
CN1CCN(c2cc(I)c(N(C)C(=O)C(C)(C)c3cc(C(F)(F)F)cc(C(F)(F)F)c3)cn2)CC1
title compound
المردود 31.0%
CN1CCN(c2cc(I)c(N(C)C(=O)C(C)(C)c3cc(C(F)(F)F)cc(C(F)(F)F)c3)cn2)CC1
2-(3,5-Bis-trifluoromethyl-phenyl)-N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-N-methyl-isobutyramide
المردود 31.0%

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added
  2. 2
    تركيزThe reaction mixture was concentrated in vacuo
  3. 3
    أخرىpurified by flash chromatography

الإجراء التجريبي

To a solution of 3.09 g (5.15 mmol) 2-(3,5-bis-trifluoromethyl-phenyl)-N-[4-iodo-6-(4-methyl-piperazin-1-yl)-pyridin-3-yl]-isobutyramide in 30 ml N,N-dimethylformamide were added at 0° C. 6.8 ml (6.2 mmol) of a 0.91 M solution of potassium bis(trimethylsilyl)amide in tetrahydrofuran. After stirring at 0° C. for 40 min 0.352 ml (5.66 mmol) iodomethane were added. The mixture was stirred for 2 days in a closed flask. The reaction mixture was concentrated in vacuo and purified by flash chromatography to give 980 mg (31%) of the title compound as a brown oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07211579B2uspto-grants-2007_05