Phosphorus oxide (P4O10) → 2-Methyl-2,3-dihydro-1,4-benzodioxine-2-carbonitrile
반응식
[CH3:1][C:2]1([C:12]([NH2:14])=O)[O:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4][CH2:3]1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C1(C)C=CC=CC=1>[C:12]([C:2]1([CH3:1])[O:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4][CH2:3]1)#[N:14]참가 물질
4
실험 절차
A stirred mixture of 2-methyl-1,4-benzodioxan-2-carboxamide (8.17 g), phosphorus pentoxide (17 g) and anhydrous toluene (175 ml) was heated under reflux for 4 hours. On cooling the supernatant was decanted from the residue, the latter being washed by decantation with more toluene. Filtration and evaporation of the solvent gave a solid residue (5.18 g). Crystallisation from ethanol yielded the cyano compound (4.4 g); m.p. 88°-89°.
후처리
- temperaturewas heated
- temperatureunder reflux for 4 hours
- temperatureOn cooling the supernatant
- customwas decanted from the residue
- washthe latter being washed by decantation with more toluene
- filtrationFiltration and evaporation of the solvent
출처 및 근거
- ORD 기록
- ord-d2293c3eeb2f4f1a884dea80100370e0
- 출처 데이터셋
- uspto-grants-1983_08
- 특허 번호
- US04397860
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