Hydrochloric Acid → 1,1'-Oxybis[2-(2-chloroethoxy)ethane]

HRID 2049104ノート

反応式

HRID 2049104 の反応式
[CH2:1](O)[CH2:2][O:3][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11]O.N1C=CC=CC=1.S(Cl)([Cl:22])=O.[ClH:24]>O.C1C=CC=CC=1>[Cl:24][CH2:1][CH2:2][O:3][CH2:4][CH2:5][O:6][CH2:7][CH2:8][O:9][CH2:10][CH2:11][Cl:22]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 8200Tetraethylene GlycolHCID 24386Thionyl Chloride

生成物 1

HCID 611871,1'-Oxybis[2-(2-chloroethoxy)ethane]

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

A mixture of 430 g of tetraethylene glycol (2.2 moles), 2000 ml of dry benzene, and 386 g of pyridine (4.9 moles) is heated to reflux, and 580 g of thionyl chloride (4.9 moles) is added dropwise with stirring in three hours. During this period the reflux temperature of the mixture drops from 86° to 78°, and a white precipitate is formed. Heating is continued overnight (16 hours) and, after cooling, 50 ml of hydrochloric acid diluted with 200 ml of water is added dropwise in about 15 minutes. Benzene is removed from the upper layer containing the product, and the residue vacuum distilled at 4.5 mm Hg at 165°. The yield is 375 g of light yellow liquid (72%).

後処理

  1. temperatureis heated
  2. temperatureto reflux
  3. waitDuring this period the reflux temperature of the mixture drops from 86° to 78°
  4. customa white precipitate is formed
  5. temperatureHeating
  6. waitis continued overnight
  7. temperature(16 hours) and, after cooling
  8. additionis added dropwise in about 15 minutes
  9. customBenzene is removed from the upper layer
  10. additioncontaining the product
  11. distillationthe residue vacuum distilled at 4.5 mm Hg at 165°

出典と根拠

ORDレコード
ord-a20294d38c7f4a97a6d417e365d693e9
出典データセット
uspto-grants-1980_04
特許番号
US04196250

反応ノート

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