참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | ethyl phosphonothioic dichloride, anhydrous | HCID 61246 | — |
| 반응물 | 3-Sulfanylbutan-1-ol | HCID 6430893 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 2-Ethyl-1,3,2-oxathiaphosphepane 2-sulphide | HCID 20185070 | 59% |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04695563 |
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| 출처 데이터셋 | uspto-grants-1987_09 |
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| ORD ID | ord-af85d24e43d14ffea4997d3637857b2d |
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| 출처 메모 | uspto-grants-1987_09 |
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