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

HRID 1756024ノート

反応式

HRID 1756024 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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##

後処理

  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

出典と根拠

ORDレコード
ord-52e3717d16c747f6a751bb4c2d3ae354
出典データセット
uspto-grants-1995_08
特許番号
US05439909

反応ノート

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