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

HRID 1074188

반응식

HRID 1074188 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-2-carboxylate.

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-3e4bd09f64d1463bb5969599b4d6b8f4
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04973600

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