Glycol monoethyl ether → 2-(Chloroethanesulfinyloxy)ethyl 2-chloroethanesulfinate

HRID 2163428ノート

反応式

HRID 2163428 の反応式
CC[O:3][CH2:4][CH2:5][OH:6].[Cl:7][CH2:8][CH2:9][S:10](Cl)=[O:11]>CCOCC>[Cl:7][CH2:8][CH2:9][S:10]([O:6][CH2:5][CH2:4][O:3][S:10]([CH2:9][CH2:8][Cl:7])=[O:11])=[O:11]

参加物

4

反応物 2

HCID 8076Glycol monoethyl etherHCID 125500522-Chloroethanesulfinic chloride

生成物 1

HCID 541517392-(Chloroethanesulfinyloxy)ethyl 2-chloroethanesulfinate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Ethyl glycol (6.2) was added dropwise under a nitrogen atmosphere to a stirred solution of 2-chloroethanesulfinyl chloride (14.7 w), prepared as in Example I, in dry ether (40 v). During the addition period the temperature of the reaction was controlled at -20° by external cooling. Upon completion of the addition, the reaction mixture was warmed to ambient temperature and the solvent was removed by distillation in a vacuum. Examination of the residue by gas-liquid chromatography revealed more than one major component. The residue was then redissolved in dry ether (200 v) and further treated with 2-chloroethanesulfinyl chloride (14.7 w) as above. Using the same procedure as above an oily residue was obtained which after purification in a wiped film molecular still yielded a colorless liquid, 2-(chloroethanesulfinyloxy)ethyl 2-chloroethanesulfinate (8.5 w) boiling at 110-115° under reduced pressure (1 × 10-4 torr).

後処理

  1. additionDuring the addition period the temperature of the reaction
  2. customwas controlled at -20° by external cooling
  3. additionUpon completion of the addition
  4. customthe solvent was removed by distillation in a vacuum
  5. dissolutionThe residue was then redissolved in dry ether (200 v)
  6. additionfurther treated with 2-chloroethanesulfinyl chloride (14.7 w) as above
  7. customwas obtained which
  8. customafter purification in a wiped film molecular still

出典と根拠

ORDレコード
ord-1ea2fb48474240e0aa750c38425de706
出典データセット
uspto-grants-1979_01
特許番号
US04134752

反応ノート

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