Allyl bromide → HCID 21857121, 화합물

HRID 1383426노트

반응식

HRID 1383426 반응식
[CH2:1](Br)[CH:2]=[CH2:3].[F:5][C:6]1[C:7](=[O:19])[O:8][C:9]2[C:14]([C:15]=1[CH3:16])=[CH:13][CH:12]=[C:11]([OH:17])[C:10]=2[CH3:18].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[F:5][C:6]1[C:7](=[O:19])[O:8][C:9]2[C:14]([C:15]=1[CH3:16])=[CH:13][CH:12]=[C:11]([O:17][CH2:3][CH:2]=[CH2:1])[C:10]=2[CH3:18]

참가 물질

5

반응물 3

HCID 7841Allyl bromide2회HCID 11430Potassium CarbonateHCID 10798396HCID 10798396, 화합물

생성물 1

HCID 21857121HCID 21857121, 화합물수율 78%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Allyl bromide (1.08 mL, 12.48 mmoles) was added to a mixture of 3-fluoro-4,8-dimethyl-7-hydroxycoumarin (1.73 g, 8.31 mmoles), ca. 5 g of potassium carbonate and 45 mL of dry acetone. The reaction mixture was stirred under an inert atmosphere at room temperature for 28 hours. During this time, excess allyl bromide (1.44 mL, 16.64 mmoles) was added in two portions. The carbonate salt was removed by suction filtration washed with acetone and the solvent evaporated under reduced pressure yielding a solid, which was purified by recrystallisation from a mixture of methanol:water. Thus, 1.60 g (78% yield) of 3-fluoro-4,8-dimethyl-7-allyloxycoumarin was obtained as a white solid: mp 117° C.

후처리

  1. customThe carbonate salt was removed by suction filtration
  2. washwashed with acetone
  3. customthe solvent evaporated under reduced pressure
  4. customyielding a solid, which
  5. customwas purified by recrystallisation from a mixture of methanol

출처 및 근거

ORD 기록
ord-2916b82184b5426d95cf375df2ee0c68
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255324B1

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