Benzenesulfinyl chloride → HCID 54259655、化合物

HRID 745805

反応式

HRID 745805 の反応式
[CH2:1]([O:3][C:4]([CH:6]1[O:10][C:9]2[CH:11]=[CH:12][C:13]([CH3:15])=[CH:14][C:8]=2[O:7]1)=[O:5])[CH3:2].[C:16]1([S:22](Cl)=[O:23])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl.ClC(Cl)C>[CH2:1]([O:3][C:4]([CH:6]1[O:7][C:8]2[CH:14]=[C:13]([CH3:15])[C:12]([S:22]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[O:23])=[CH:11][C:9]=2[O:10]1)=[O:5])[CH3:2]

参加物

6

反応物 3

HCID 4190003Benzenesulfinyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 54313136HCID 54313136、化合物

生成物 1

HCID 54259655HCID 54259655、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒HCID 63651,1-Dichloroethane溶媒

実験手順

20.8 g (0.1 mol) of 5-methyl-1,3-benzodioxole-2-carboxylic acid ethyl ester Example 2b) and 19.2 g (0.125 mol) of phenylsulphinic acid chloride are dissolved in 200 ml of 1,2-dichloroethane and cooled to 5° using an ice-bath. 13.3 g (0.1 mol) of aluminium chloride are introduced in the course of approximately 15 minutes at from 5°-10° while stirring. The mixture is stirred for a further hour in the ice-bath and is then poured out onto ice-water. The resulting emulsion is diluted with 200 ml of dichloroethane and filtered across a layer of a filter aid (for example Hyflo). The filtrate is introduced into a separating funnel and the layers are separated. The organic phase is dried over sodium sulphate, filtered and concentrated to dryness by evaporation. A light brown honey-like product, 5-phenylsulphinyl-6-methyl-1,3-benzodioxole-2-carboxylic acid ethyl ester, is obtained.

後処理

  1. temperaturecooled to 5°
  2. additionis then poured out onto ice-water
  3. additionThe filtrate is introduced into a separating funnel
  4. customthe layers are separated
  5. dry with materialThe organic phase is dried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness by evaporation

出典と根拠

ORDレコード
ord-3626516582ce4e578fbdc7089df2579f
出典データセット
uspto-grants-1986_07
特許番号
US04600709

関連ノート

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