Sodium → HCID 21311730, 화합물

HRID 971824노트

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HRID 971824 반응식
[Na].[C:2]1([CH:8]([OH:11])[CH2:9][SH:10])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:12]([CH:14](Cl)[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH2:13]>C1(C=CC(O)=CC=1)O.C(O)C>[C:2]1([CH:8]([OH:11])[CH2:9][S:10][CH:14]([CH:12]=[CH2:13])[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 5360545Sodium2회HCID 11768772Benzene, 1-(chloromethyl)-3(or 4)-ethenyl-HCID 120486141-phenyl-2-sulfanylethan-1-ol

생성물 1

HCID 21311730HCID 21311730, 화합물수율 104.8%

시약·촉매·용매 2

HCID 785Hydroquinone촉매HCID 702Ethanol용매

실험 절차

To 125 ml of absolute ethanol was added 5.7 g (0.247 moles) of sodium metal. After the sodium had dissolved, the solution was cooled to 0° to 5° C. and 38 g (0.247 moles) of 1-phenyl-2-mercaptoethanol was added dropwise. After addition, the reaction was stirred at 0° to 5° C. for 1 hour and then 37.7 g (0.247 moles) of vinylbenzyl chloride was added dropwise. After the addition was complete, 0.5 g of hydroquinone was added and the mixture was refluxed for 2 hours. The mixture was cooled and the sodium chloride was removed by filtration. The solvent was evaporated and the residue was added to 100 ml of water. The aqueous mixture was extracted with three 100 ml portions of ether and the combined ethereal extracts were dried over anhydrous magnesium sulfate, filtered, and the solvent evaporated to leave 70 g of the product as a crude oil. Due to its high boiling point, the product was used without further purification in the synthesis of the following sulfone.

후처리

  1. temperaturethe solution was cooled to 0° to 5° C.
  2. additionAfter addition
  3. additionAfter the addition
  4. temperaturethe mixture was refluxed for 2 hours
  5. temperatureThe mixture was cooled
  6. customthe sodium chloride was removed by filtration
  7. customThe solvent was evaporated
  8. additionthe residue was added to 100 ml of water
  9. extractionThe aqueous mixture was extracted with three 100 ml portions of ether
  10. dry with materialthe combined ethereal extracts were dried over anhydrous magnesium sulfate
  11. filtrationfiltered
  12. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-b1d768ecc4c841f4b872a4d82e60c010
출처 데이터셋
uspto-grants-1979_07
특허 번호
US04161407

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