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

HRID 259272ノート

反応式

HRID 259272 の反応式
[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

参加物

5

反応物 3

HCID 18430EpibromohydrinHCID 24758Sodium hydrideHCID 782524-Methylbenzyl mercaptan

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-785573d3478846f68223b52921277ede
出典データセット
uspto-grants-1977_07
特許番号
US04036970

反応ノート

読み込み中…