Hydrochloric Acid → Ethyl 6-acetyl-1,4-benzodioxin-2-carboxylate

HRID 1756024노트

반응식

HRID 1756024 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:7])[CH3:6].[O:9]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[O:12][CH:11]=[C:10]1[C:19]([O:21][CH2:22][CH3:23])=[O:20].Cl>C(=S)=S>[C:5]([C:17]1[CH:16]=[CH:15][C:14]2[O:9][C:10]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:11][O:12][C:13]=2[CH:18]=1)(=[O:7])[CH3:6]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 10987416Ethyl 1,4-benzodioxin-2-carboxylate

생성물 1

HCID 11806994Ethyl 6-acetyl-1,4-benzodioxin-2-carboxylate수율 95%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

Slowly add 8.1 g (60.7 mmol) of aluminium chloride to a solution of 2.85 g (36.3 mmol) of acetyl chloride and 5 g (24.7 mmol) of ethyl 1,4-benzodioxin-2-carboxylate in 120 cm3 of carbon disulfide at 0° C. Stir for 4 hours at room temperature and then, after acid hydrolysis with 20 cm3 of 2N hydrochloric acid, extract the reaction mixture with methylene chloride. After drying the methylene chloride phase over magnesium sulfate, concentrating to dryness and washing with ethanol, ethyl 6-acetyl-1,4-benzodioxin-2-carboxylate is obtained in a yield of 95%. Melting point: 122° C. ##STR30##

후처리

  1. customat 0° C
  2. extractionextract the reaction mixture with methylene chloride
  3. dry with materialAfter drying the methylene chloride phase over magnesium sulfate
  4. concentrationconcentrating to dryness
  5. washwashing with ethanol

출처 및 근거

ORD 기록
ord-52e3717d16c747f6a751bb4c2d3ae354
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05439909

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