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

HRID 1105587
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HRID 1105587 반응식
[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]
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참가 물질

5

반응물 3

HCID 6998SalicylaldehydeHCID 8471TriethylamineHCID 57142200S-ethyl S-propyl chlorotrithiophosphate

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8081d7d64a0c47b69aa32cca630b553a
출처 데이터셋
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04309422

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