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Dimethyl Sulfate → 2-Methoxy-3-(2-chlorophenylthio)benzaldehyde

HRID 1164078
ノート
印刷プレビュー

反応式

HRID 1164078 の反応式
[OH:1][C:2]1[C:9]([S:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5].S(OC)(O[CH3:22])(=O)=O>[OH-].[K+]>[CH3:22][O:1][C:2]1[C:9]([S:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[CH:8][CH:7]=[CH:6][C:3]=1[CH:4]=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6497Dimethyl SulfateHCID 205134432-Hydroxy-3-(2-chlorophenylthio)benzaldehyde

生成物 1

HCID 205134222-Methoxy-3-(2-chlorophenylthio)benzaldehyde収率 45.3%

試薬・触媒・溶媒 1

HCID 14797Potassium Hydroxide溶媒

実験手順

A mixture of 2-hydroxy-3-(2-chlorophenylthio)benzaldehyde (19.3 g) and dimethyl sulfate (18.4 g) was stirred at room temperature. To the mixture was added dropwise an aqueous solution (50 ml) of potassium hydroxide (12.5 g) at temperature below 60° C., and then the mixture was stirred for an hour. The reaction mixture was cooled to the ambient temperature and insoluble substance was filtered off. The filtrate was extracted with diethyl ether, and the extract was washed with water, dried over magnesium sulfate and then evaporated under reduced pressure to give oily 2-methoxy-3-(2-chlorophenylthio)benzaldehyde (9.2 g).

後処理

  1. stirringthe mixture was stirred for an hour
  2. temperatureThe reaction mixture was cooled to the ambient temperature and insoluble substance
  3. filtrationwas filtered off
  4. extractionThe filtrate was extracted with diethyl ether
  5. washthe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-8fd23be2987848789d8e31e8d523dfd2
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04367238

反応ノート

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