関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,4-Dimethylphenol | HCID 7771 | — |
| 反応物 | Thiophosphoryl chloride | HCID 19883 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | Bis(2,4-dimethylphenyl) chlorothiophosphate | HCID 19690204 | 89.9% |
反応手順
Thiophosphoryl chloride (17.0 g) was dissolved in tuoluene (250 cm3) and triethylamine (21.5 g) was added. The solution was stirred at 20° C. and 2,4-dimethylphenol (24.4 g) was added in portions during 1 hr. The mixture was stirred for 2 hr. and then heated and stirred at 80° C. for a further 2 hr. and then cooled and filtered to remove thriethylamine hydrochloride. The toluene was distilled under reduced pressure leaving bis(2,4-dimethylphenyl) chlorothiophosphate (oil, 30.6 g. 31P NMR in CDCl3, singlet 54.57 ppm downfield of H3 PO4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05728853 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-0308ebab0a1b4896a483600b07def253 |
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| 出典メモ | uspto-grants-1998_03 |
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