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

HRID 2309364

反応式

HRID 2309364 の反応式
[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]

参加物

7

反応物 5

HCID 962WaterHCID 1140Toluene2 回HCID 8471TriethylamineHCID 61246ethyl phosphonothioic dichloride, anhydrousHCID 64308933-Sulfanylbutan-1-ol

生成物 1

HCID 201850702-Ethyl-1,3,2-oxathiaphosphepane 2-sulphide収率 59%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af85d24e43d14ffea4997d3637857b2d
出典データセット
uspto-grants-1987_09
特許番号
US04695563

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