Water → 2-Ethyl-1,3,2-oxathiaphosphepane 2-sulphide

HRID 2309364

반응식

HRID 2309364 반응식
[CH2:1]([P:3](Cl)(Cl)=[S:4])[CH3:2].[SH:7]C(C)CCO.C(N(CC)CC)C.[OH2:20].[C:21]1(C)C=C[CH:24]=[CH:23][CH:22]=1>O1CCCC1>[CH2:1]([P:3]1(=[S:4])[S:7][CH2:24][CH2:23][CH2:22][CH2:21][O:20]1)[CH3:2]

참가 물질

7

반응물 5

HCID 962WaterHCID 1140Toluene2회HCID 8471TriethylamineHCID 61246ethyl phosphonothioic dichloride, anhydrousHCID 64308933-Sulfanylbutan-1-ol

생성물 1

HCID 201850702-Ethyl-1,3,2-oxathiaphosphepane 2-sulphide수율 59%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
80 °C

실험 절차

16.3 g (0.1 mol) of ethanethiophosphonic dichloride in 1 l of toluene are initially introduced, and a mixture of 11 g (0.1 mol) of 3-mercaptobutan-1-ol and 22 g (0.22 mol) of triethylamine in 100 ml of tetrahydrofuran is slowly added dropwise at 20° C. The mixture is heated at 80° C. for 2 days, and 200 ml of toluene and 200 ml of water are then added to the reaction mixture. The organic phase is separated off, washed with water and dried, and the solvent is distilled off, first under a vacuum from a waterpump and then under a high vacuum. 11.5 g (59 % of theory) of 2-ethyl-1,3,2-oxathiaphosphepane 2-sulphide having a refractive index nD20 =1.5761 are obtained.

후처리

  1. additionis slowly added dropwise at 20° C
  2. customThe organic phase is separated off
  3. washwashed with water
  4. customdried
  5. distillationthe solvent is distilled off, first under a vacuum from a waterpump

출처 및 근거

ORD 기록
ord-af85d24e43d14ffea4997d3637857b2d
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04695563

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