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Sodium Hydroxide → HCID 86735169、化合物

HRID 2419908
ノート
印刷プレビュー

反応式

HRID 2419908 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([OH:14])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[OH-].[Na+:16].Cl[CH2:18][S:19]([O-:22])(=[O:21])=[O:20].[Na+]>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([O:14][CH2:18][S:19]([O-:22])(=[O:21])=[O:20])=[CH:10][CH:9]=2)=[CH:6][CH:7]=1.[Na+:16]
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 3

HCID 14798Sodium HydroxideHCID 915894'-Chloro-4-biphenylolHCID 23705445chloromethanesulfonic acid

生成物 1

HCID 86735169HCID 86735169、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
80 °C

実験手順

In a 1-liter round-bottomed flask is placed 4-(4-chlorophenyl)phenol (25.5 g.), 4.0 N aqueous sodium hydroxide (39.0 ml.) and water (75 ml.). The mixture is heated to 90°-100° C., and sodium chloromethyl sulphonate (46.5 g.) is added. The mixture is heated rapidly to 160°-170° C. (bath temperature) while a current of air is passed through the flask. When most of the water has been removed the temperature of the bath is raised to, and kept at, 220°-225° C., for 90 minutes; the mixture is then cooled. The solid cakes obtained from two identical experiments are ground with water (200 ml.) in a mortar. The resulting suspension is heated to 80° C. and allowed to cool slowly, then filtered. The product is washed with water and dried to give sodium 4-(4-chlorophenyl)phenoxymethylsulphonate (58.4 g.) as a cream coloured powder pure enough for use. It may be further purified by crystallisation from aqueous dimethylsulphoxide and obtained as a microcrystalline powder not melting at 300° C.

後処理

  1. customIn a 1-liter round-bottomed flask is placed
  2. temperatureThe mixture is heated to 90°-100° C.
  3. temperatureThe mixture is heated rapidly to 160°-170° C. (bath temperature) while a current of air
  4. customWhen most of the water has been removed the temperature of the bath
  5. temperatureis raised to, and
  6. custom220°-225° C.
  7. temperaturethe mixture is then cooled
  8. customThe solid cakes obtained from two identical experiments
  9. temperatureto cool slowly
  10. filtrationfiltered
  11. washThe product is washed with water
  12. customdried

出典と根拠

ORDレコード
ord-89e57e301cd04dcdb17e40394bb84daa
出典データセット
uspto-grants-1978_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04107329

反応ノート

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