Sodium Chloride → 2-Dodecylbenzene-1-sulfonyl chloride

HRID 464241

反応式

HRID 464241 の反応式
[CH2:1]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[S:19]([OH:22])(=O)=[O:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].C(OCC)(=O)C.P(Cl)(Cl)([Cl:31])=O.[Cl-].[Na+]>O.CN(C)C=O>[CH2:1]([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[S:19]([Cl:31])(=[O:22])=[O:20])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

参加物

7

反応物 4

HCID 5234Sodium ChlorideHCID 8857Ethyl AcetateHCID 24813Phosphorus oxychlorideHCID 25457Dodecylbenzenesulphonic acid

生成物 1

HCID 204390012-Dodecylbenzene-1-sulfonyl chloride

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution composed of 32.7 g (0.1 mol) of dodecylbenzenesulfonic acid, 80 ml of ethyl acetate, and 12 ml of dimethylformamide (DMF) was added dropwise 12.4 ml (0.15 mol) of phosphorus oxychloride with stirring over a period of 10 minutes and then while heating the mixture so as to maintain the temperature thereof at 40° C., the reaction was performed for 60 minutes. After the reaction was over, the reaction mixture was cooled to 5° to 10° C. and then a solution composed of 16 g of sodium chloride and 160 ml of water was added dropwise to the reaction mixture over a period of 15 minutes. After removing an aqueous layer, an ethyl acetate layer thus formed was washed once with 100 ml of an aqueous 10% sodium chloride solution. The ethyl acetate solution of dodecylbenzenesulfonyl chloride obtained was used for the subsequent reaction as it was.

後処理

  1. temperaturewhile heating the mixture so as
  2. temperatureto maintain the temperature
  3. waitat 40° C., the reaction was performed for 60 minutes
  4. temperaturewas cooled to 5° to 10° C.
  5. additionwas added dropwise to the reaction mixture over a period of 15 minutes
  6. customAfter removing an aqueous layer
  7. customan ethyl acetate layer thus formed
  8. washwas washed once with 100 ml of an aqueous 10% sodium chloride solution

出典と根拠

ORDレコード
ord-3512c7e676b14115b288d83f8d6f60e5
出典データセット
uspto-grants-1985_10
特許番号
US04547452

関連ノート

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