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

HRID 1158707

반응식

HRID 1158707 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ce58f09de14b471cae6210ff0e695b82
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812025B2

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