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Salicylaldehyde → S-Ethyl S-Propyl O-(2-Formylphenyl) Trithiophosphate

HRID 1105587
ノート
印刷プレビュー

反応式

HRID 1105587 の反応式
[P:1](Cl)([S:6][CH2:7][CH2:8][CH3:9])([S:3][CH2:4][CH3:5])=[S:2].C(N(CC)CC)C.[OH:18][C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=[O:22]>C(Cl)Cl>[P:1]([O:18][C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=[O:22])([S:6][CH2:7][CH2:8][CH3:9])([S:3][CH2:4][CH3:5])=[S:2]
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 6998SalicylaldehydeHCID 8471TriethylamineHCID 57142200S-ethyl S-propyl chlorotrithiophosphate

生成物 1

HCID 57137846S-Ethyl S-Propyl O-(2-Formylphenyl) Trithiophosphate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

反応条件

温度
0 °C

実験手順

A solution of S-ethyl S-propyl chlorotrithiophosphate (0.03 mole) in methylene chloride (50 ml) is charged into a glass reaction vessel equipped with a mechanical stirrer. Triethylamine (0.03 mole) is added and the mixture is cooled to a temperature of about 0° C. A solution of 2-hydroxybenzaldehyde (0.03 mole) in methylene chloride (15 ml) is slowly added with stirring while maintaining the temperature of the reaction mixture at about 0° C. After the addition is completed the reaction mixture is allowed to warm to room temperature and stirring is continued for a period of about 1 hour. After this time the reaction mixture is transferred to a separatory funnel and methylene chloride (100 ml) is added. The resulting solution is then washed with water, dilute aqueous sodium hydroxide and again with water. The washed solution is dried over anhydrous magnesium sulfate, is filtered and stripped of solvent under vacuum to yield the desired product S-ethyl S-propyl O-(2-formylphenyl)trithiophosphate.

後処理

  1. customequipped with a mechanical stirrer
  2. temperaturewhile maintaining the temperature of the reaction mixture at about 0° C
  3. additionAfter the addition
  4. temperatureto warm to room temperature
  5. stirringstirring
  6. customAfter this time the reaction mixture is transferred to a separatory funnel
  7. washThe resulting solution is then washed with water, dilute aqueous sodium hydroxide and again with water
  8. dry with materialThe washed solution is dried over anhydrous magnesium sulfate
  9. filtrationis filtered

出典と根拠

ORDレコード
ord-8081d7d64a0c47b69aa32cca630b553a
出典データセット
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04309422

反応ノート

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