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Phosphorus tribromide → 5-(Bromomethyl)-3-dodecylisoxazole

HRID 264105
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반응식

HRID 264105 반응식
[CH2:1]([C:13]1[CH:17]=[C:16]([CH2:18]O)[O:15][N:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].P(Br)(Br)[Br:21]>ClCCl>[Br:21][CH2:18][C:16]1[O:15][N:14]=[C:13]([CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 106355535-Isoxazolemethanol, 3-dodecyl-

생성물 1

HCID 105443765-(Bromomethyl)-3-dodecylisoxazole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred, chilled (+3° C.) solution of 3-dodecyl-5-isoxazole methanol (1.0 g, 0.0037 mol) in dichloromethane (20 mL) was added in one portion phosphorous tribromide (0.13 mL, 0.0014 mol), and the solution was stirred at +3° C. for 1.5 hours, then at room temperature for 3 days. The mixture was washed carefully with saturated sodium bisulfite, saturated sodium bicarbonate, and saturated sodium chloride. The organic layer was dried (MgSO4) and rotoevaporated to a yellow oil which solidified upon standing; yield 1.12 g (93%); mp 31.5°-35° C.

후처리

  1. waitat room temperature for 3 days
  2. washThe mixture was washed carefully with saturated sodium bisulfite, saturated sodium bicarbonate, and saturated sodium chloride
  3. dry with materialThe organic layer was dried (MgSO4)

출처 및 근거

ORD 기록
ord-9853026feefe4cb884172586f796507f
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05646170

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