2-Bromo-4-phenylpyridine → Tert-butyl 4-(4-phenylpyridin-2-yl)piperazine-1-carboxylate

HRID 1158707

反応式

HRID 1158707 の反応式
Br[C:2]1[CH:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:5]=[CH:4][N:3]=1.[C:14]([O:18][C:19]([N:21]1[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1)=[O:20])([CH3:17])([CH3:16])[CH3:15]>N1C=CC=CC=1>[C:8]1([C:6]2[CH:5]=[CH:4][N:3]=[C:2]([N:24]3[CH2:23][CH2:22][N:21]([C:19]([O:18][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:20])[CH2:26][CH2:25]3)[CH:7]=2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 1047002-Bromo-4-phenylpyridineHCID 143452tert-Butyl piperazine-1-carboxylate

生成物 1

HCID 68644576Tert-butyl 4-(4-phenylpyridin-2-yl)piperazine-1-carboxylate収率 20.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2-bromo-4-phenylpyridine (1.34 g, 5.72 mmol), 1-(tert-butoxycarbonyl)piperazine (3.19 g, 17.2 mmol) and pyridine (20 ml) was stirred at 125° C. for 7 days, and the solvent was distilled away under reduce pressure. To the residue was added water, and extracted with ethyl acetate. The extract was washed with water, and the solvent was distilled away under reduce pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1) to give the titled compound 390 mg (20.1%) as solid product.

後処理

  1. distillationthe solvent was distilled away
  2. additionTo the residue was added water
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with water
  5. distillationthe solvent was distilled away
  6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-ce58f09de14b471cae6210ff0e695b82
出典データセット
uspto-grants-2010_10
特許番号
US07812025B2

関連ノート

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