関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 6H-Dibenz[c,e][1,2]oxaphosphorin, 6-chloro- | HCID 89816 | — |
| 生成物 | CID 37314 | HCID 37314 | 100% |
反応手順
77.6 g (0.331 mol) of 6-chloro-(6H)-dibenzo[c,e][1,2]oxaphosphorin are heated to 110° C. 5.96 g (0.331 mol) of water are subsequently added over the course of 30 minutes with vigorous stirring, during which some of the hydrogen chloride gas produced departs. The temperature is subsequently raised in steps to 180° C. and is maintained until no further hydrogen chloride is evolved (a period of approximately 2 hours). The reaction product is subsequently cooled, solidifies, and is comminuted. 71.5 g of 6H-dibenzo[c,e][1,2]-oxaphosphorin-6-one (melting point: 117° C.) are obtained, corresponding to a yield of 100 % of theory. In accordance with 31P NMR spectroscopy the purity is 99%, and the content of hydrogen chloride is 0.08%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05481017 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-d4cb6159c8a94848bb0e1e8c1a850742 |
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| 出典メモ | uspto-grants-1996_01 |
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