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N-[4-Cyano-3-(trifluoromethyl)phenyl]-2-methyloxirane-2-carboxamide → Bicalutamide

HRID 457265
ノート
印刷プレビュー

反応式

HRID 457265 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([C:12]2([CH3:15])[CH2:14][O:13]2)=[O:11])=[CH:5][C:4]=1[C:16]([F:19])([F:18])[F:17])#[N:2].[F:20][C:21]1[CH:26]=[CH:25][C:24]([S:27]([O-:29])=[O:28])=[CH:23][CH:22]=1.[Na+]>C(Cl)(Cl)Cl.O.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH3:15][C:12]([OH:13])([C:10]([NH:9][C:6]1[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[C:4]([C:16]([F:19])([F:18])[F:17])[CH:5]=1)=[O:11])[CH2:14][S:27]([C:24]1[CH:23]=[CH:22][C:21]([F:20])=[CH:26][CH:25]=1)(=[O:29])=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 10149314N-[4-Cyano-3-(trifluoromethyl)phenyl]-2-methyloxirane-2-carboxamideHCID 236662204-fluorobenzenesulfinic acid sodium salt

生成物 1

HCID 2375Bicalutamide

試薬・触媒・溶媒 3

HCID 74236Tetrabutylammonium Bromide触媒HCID 962Water溶媒HCID 6212
Chloroform
溶媒
2 回

実験手順

0.500 g of the epoxyamide (5A) was dissolved in a mixture of 40 ml of chloroform and 40 ml of water and 371 mg of sodium p-fluorobenzenesulfinate was added. Subsequently, 298 mg of tetrabutylammonium bromide was added. The reaction mixture was heated till reflux, while stirring vigorously. The reaction was monitored with HPLC. After 96 hours of reflux, the reaction mixture was cooled to room temperature. 20 ml of chloroform was added and the organic layer was washed with 3×50 ml of water, dried (Na2SO4) and evaporated to dryness. Yield: 860 mg. Purification of the crude product by column chromatography (Merck silica gel 60; eluent: heptane/ethyl acetate=1/1) afforded bicalutamide as white solid. Isolated yield: 380 mg (48%). 1H-NMR: confirmed the structure.

後処理

  1. additionwas added
  2. temperatureThe reaction mixture was heated
  3. temperaturetill reflux
  4. temperatureAfter 96 hours of reflux
  5. washthe organic layer was washed with 3×50 ml of water
  6. dry with materialdried (Na2SO4)
  7. customevaporated to dryness
  8. customPurification of the crude product by column chromatography (Merck silica gel 60; eluent: heptane/ethyl acetate=1/1)

出典と根拠

ORDレコード
ord-fcbf07e29a3d498683bd5248bede777c
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07186854B2

反応ノート

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