Phenyl isocyanate → HCID 178493809, 화합물
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[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[O:8]C.N1CCOCC1.C1(N=C=O)C=CC=CC=1>C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([O:10][CH3:11])[C:7]=1[OH:8]참가 물질
5
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- 온도
- 0 °C
실험 절차
3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr and the mixture was cooled to 0° C. To the reaction mixture was added phenyl isocyanate (73.8 mL) at 0° C., and the mixture was stirred at the same temperature for 30 min and diluted with ethyl acetate. The resulting N-phenylmorpholine-4-carboxamide was removed by filtration. The filtrate was concentrated and purified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate) to give the title compound (9.61 g).
후처리
- customThe resulting N-phenylmorpholine-4-carboxamide was removed by filtration
- concentrationThe filtrate was concentrated
- custompurified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate)
출처 및 근거
- ORD 기록
- ord-1ac729433b494861add832116a75e4a7
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09150588B2
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