Epibromohydrin → 1,3-Bis(4'-methylbenzylthio)-2-propanol

HRID 259272노트

반응식

HRID 259272 반응식
[CH2:1]([CH:3]1[O:5][CH2:4]1)Br.[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([CH2:11][SH:12])=[CH:9][CH:8]=1.[H-].[Na+]>O1CCCC1>[CH3:6][C:7]1[CH:14]=[CH:13][C:10]([CH2:11][S:12][CH2:1][CH:3]([OH:5])[CH2:4][S:12][CH2:11][C:10]2[CH:13]=[CH:14][C:7]([CH3:6])=[CH:8][CH:9]=2)=[CH:9][CH:8]=1

참가 물질

5

반응물 3

HCID 18430EpibromohydrinHCID 24758Sodium hydrideHCID 782524-Methylbenzyl mercaptan

생성물 1

HCID 214237301,3-Bis(4'-methylbenzylthio)-2-propanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

Epibromohydrin (1.37 g.) in 2 ml. dry tetrahydrofuran is added to a stirred suspension of the salt obtained by mixing 3 g. of 4-methylbenzyl mercaptan and 550 mg. of sodium hydride (56% dispersion in mineral oil) in 60 ml. dry tetrahydrofuran. The resulting solution is heated at reflux for 4 hours. Thereafter, the solvent is removed and 30 ml. of water is added to the residue. The resultant aqueous mixture is extracted with ether and the ether extracts washed with water, dried over magnesium sulfate and evaporated to dryness to yield 1,3-bis(4'-methylbenzylthio)-2-propanol.

후처리

  1. customobtained
  2. additionby mixing 3 g
  3. temperatureThe resulting solution is heated
  4. temperatureat reflux for 4 hours
  5. customThereafter, the solvent is removed
  6. additionof water is added to the residue
  7. extractionThe resultant aqueous mixture is extracted with ether
  8. washthe ether extracts washed with water
  9. dry with materialdried over magnesium sulfate
  10. customevaporated to dryness

출처 및 근거

ORD 기록
ord-785573d3478846f68223b52921277ede
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036970

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