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Acetic Acid → Methyl [p-(p-chlorophenylsulfonyl)phenyl]acetate

HRID 1704036
ノート
印刷プレビュー

反応式

HRID 1704036 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([O:18][CH3:19])=[O:17])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.C(O)(=[O:22])C.OO.[OH2:26]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([O:18][CH3:19])=[O:17])=[CH:11][CH:10]=2)(=[O:22])=[O:26])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 962WaterHCID 12531842Methyl [p-(p-chlorophenylthio)phenyl]acetate

生成物 1

HCID 53805964Methyl [p-(p-chlorophenylsulfonyl)phenyl]acetate

反応条件

温度
70 °C

実験手順

A mixture of 14.62 g of methyl [p-(p-chlorophenylthio)phenyl]acetate, 100 ml of glacial acetic acid and 62.5 ml of 30% hydrogen peroxide is heated to 70° C and kept at 70° C for 3 hours. After cooling, the mixture is poured into 500 ml of water and extracted with three 100 ml portions of chloroform. The combined extracts are washed with three 100 ml portions of water, 100 ml of saturated NaHCO3, saturated brine and dried over MgSO4. Evaporation of the solvent affords an oil which crystallizes on standing to give 14.9 g of product as white crystals (from petroleum ether) mp 78°-80° C.

後処理

  1. temperatureAfter cooling
  2. extractionextracted with three 100 ml portions of chloroform
  3. washThe combined extracts are washed with three 100 ml portions of water, 100 ml of saturated NaHCO3, saturated brine
  4. dry with materialdried over MgSO4
  5. customEvaporation of the solvent
  6. customaffords an oil which
  7. customcrystallizes

出典と根拠

ORDレコード
ord-a92c527f623d467baec3f4c5dfccee86
出典データセット
uspto-grants-1978_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04125729

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート