Potassium Carbonate → Ethyl 4,5-dichloro-1,3-benzodioxole-2-carboxylate

HRID 1089171

반응식

HRID 1089171 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[C:4]([OH:9])[C:3]=1[OH:10].C(=O)([O-])[O-].[K+].[K+].Br[CH:18](Br)[C:19]([O:21][CH2:22][CH3:23])=[O:20]>CN(C)C=O>[Cl:1][C:2]1[C:3]2[O:10][CH:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[O:9][C:4]=2[CH:5]=[CH:6][C:7]=1[Cl:8]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 198773,4-DichlorocatecholHCID 69237Ethyl dibromoacetate

생성물 1

HCID 14748637Ethyl 4,5-dichloro-1,3-benzodioxole-2-carboxylate수율 66.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

A mixture of 11.0 g of 3,4-dichloro-1,2-benzenediol, 15.38 g of potassium carbonate, 27 g of ethyl dibromoacetate and 100 ml of dimethylformamide is stirred at 100° C. under argon gas atmosphere for 4 hours. The reaction mixture is evaporated to remove solvent and ethyl acetate and water is added to the residue. The organic layer is separated, washed with water, dried and evaporated to remove solvent. The residue is purified by silica gel column chromatography to give 10.75 g of ethyl 4,5-dichloro-1,3-benzodioxole-2carboxylate.

후처리

  1. customThe reaction mixture is evaporated
  2. customto remove solvent and ethyl acetate and water
  3. additionis added to the residue
  4. customThe organic layer is separated
  5. washwashed with water
  6. customdried
  7. customevaporated
  8. customto remove solvent
  9. customThe residue is purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-9075ba1993954ec9ab3cfa7defecb40b
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04965282

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