Carbon tetrabromide → (RS)-2-(5-(1-Bromoethyl)-isoxazol-3-yl)-pyridine

HRID 707655노트

반응식

HRID 707655 반응식
O[CH:2]([C:4]1[O:8][N:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:5]=1)[CH3:3].C(Br)(Br)(Br)[Br:16]>ClCCl>[Br:16][CH:2]([C:4]1[O:8][N:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=2)[CH:5]=1)[CH3:3]

참가 물질

4

반응물 2

HCID 11205Carbon tetrabromideHCID 44605541(RS)-2-(5-(1-Hydroxyethyl)-isoxazol-3-yl)-pyridine

생성물 1

HCID 67958649(RS)-2-(5-(1-Bromoethyl)-isoxazol-3-yl)-pyridine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
30 °C

실험 절차

To a mixture of (RS)-2-(5-(1-hydroxy-ethyl)-isoxazol-3-yl)-pyridine (0.9 gm), and triphenylphosphene (1.77 gm) in dichloromethane (20 ml) was added carbontetrabromide (6 gm) at 0° C. The reaction mixture was stirred at 30° C. over a period of 2.5 h. The reaction was monitored by TLC. The reaction was quenched by addition of water and layers were separated. Combined organic extract was washed with brine and evaporated under vacuum to provide the 1.7 gm crude mass which was purified by using silica gel column chromatography to provide title compound in 0.8 gm quantity (65%).

후처리

  1. customThe reaction was quenched by addition of water and layers
  2. customwere separated
  3. extractionCombined organic extract
  4. washwas washed with brine
  5. customevaporated under vacuum
  6. customto provide the 1.7 gm crude mass which
  7. customwas purified

출처 및 근거

ORD 기록
ord-2b4b4e6d763a479285439a77f6f2d5df
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175031B2

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