반응식
Cl[P:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[C:5]2[CH:12]=[CH:13][CH:14]=[CH:15][C:4]=2[O:3]1.[OH2:16].Cl>>[CH:12]1[C:5]2[C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=3[PH:2](=[O:16])[O:3][C:4]=2[CH:15]=[CH:14][CH:13]=1참가 물질
4
반응 조건
- 온도
- 180 °C
실험 절차
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%.
후처리
- customproduced departs
- customa period of approximately 2 hours
- temperatureThe reaction product is subsequently cooled
- customis comminuted
출처 및 근거
- ORD 기록
- ord-d4cb6159c8a94848bb0e1e8c1a850742
- 출처 데이터셋
- uspto-grants-1996_01
- 특허 번호
- US05481017
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