1,2-Dibromoethane → 8-Fluoro-2,3-dihydro-1,4-benzodioxin-6-carboxaldehyde

HRID 15308

반응식

HRID 15308 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20]Br>CN(C=O)C>[F:1][C:2]1[C:9]2[O:10][CH2:19][CH2:20][O:11][C:8]=2[CH:7]=[C:4]([CH:5]=[O:6])[CH:3]=1

참가 물질

5

반응물 3

HCID 78391,2-DibromoethaneHCID 11430Potassium CarbonateHCID 5936643-Fluoro-4,5-dihydroxybenzaldehyde

생성물 1

HCID 574231098-Fluoro-2,3-dihydro-1,4-benzodioxin-6-carboxaldehyde수율 95.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 3-fluoro-4,5-dihydroxybenzaldehyde (0.66 g, 4.2 mmol) in DMF (30 ml) was added potassium carbonate (1.15 g, 8.3 mmol) and 1,2-dibromoethane (0.72 ml, 8.3 mmol) and the resultant mixture was heated to 80° C. for 18 h before the solvent was removed under reduced pressure. The reaction mixture was then treated with dichloromethane and water. The aqueous phase was extracted twice with dichloromethane and the combined organic phases were dried and the solvent was removed under reduced pressure to give the desired compound as a cream solid (0.73 g, 95%).

후처리

  1. customwas removed under reduced pressure
  2. additionThe reaction mixture was then treated with dichloromethane and water
  3. extractionThe aqueous phase was extracted twice with dichloromethane
  4. customthe combined organic phases were dried
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-ae2de73b0a5c4c679f9b21e0b468d267
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732461B2

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