Potassium Carbonate → HCID 13723675, 화합물

HRID 1448965노트

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HRID 1448965 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([OH:10])[C:5](=[CH:7][C:8]=1[CH3:9])[OH:6].C(=O)([O-])[O-].[K+].[K+].Br[C:18](Br)([CH3:24])[C:19]([O:21][CH2:22][CH3:23])=[O:20]>CC(C)=O>[CH3:1][C:2]1[C:8]([CH3:9])=[CH:7][C:5]2[O:6][CH:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:24][O:10][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 10901348Propanoic acid, 2,2-dibromo-, ethyl esterHCID 127302874,5-Dimethylbenzene-1,2-diol

생성물 1

HCID 13723675HCID 13723675, 화합물수율 319.7%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A stirred solution of 4,5-dimethylcatechol (7.0 g.) in dry acetone (45 ml.) was heated under reflux, then potassium carbonate (5 g.) was added followed by the dropwise addition of ethyl dibromopropionate (3.5 g.). The addition procedure was repeated a further three times over 11/4 hours then the reaction was stirred under reflux for a further 33/4 hours. After cooling, the mixture was filtered, the solids washed well with acetone then the combined filtrate concentrated in vacuo. Water (35 ml.) was added, the resulting solid collected, washed with petrol then taken up in ether. The ethereal solution was washed with water, dried (Na2SO4) and evaporated in vacuo to give ethyl 6,7-dimethyl-1,4-benzodioxan-2-carboxylate (10.17 g.), m.p. 70°-71° C.

후처리

  1. temperatureunder reflux
  2. additionThe addition procedure
  3. custom4 hours
  4. temperatureunder reflux for a further 33/4 hours
  5. temperatureAfter cooling
  6. filtrationthe mixture was filtered
  7. washthe solids washed well with acetone
  8. concentrationthe combined filtrate concentrated in vacuo
  9. additionWater (35 ml.) was added
  10. customthe resulting solid collected
  11. washwashed with petrol
  12. washThe ethereal solution was washed with water
  13. dry with materialdried (Na2SO4)
  14. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-dd7618234cba4d3ea4d9b913834d861f
출처 데이터셋
uspto-grants-1980_02
특허 번호
US04188390

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