Phenyl isocyanate → HCID 178493809、化合物
反応式
[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]参加物
5
反応条件
- 温度
- 0 °C
実験手順
3-Chloro-4,5-dimethoxypyridazine (17.0 g) and morpholine (59.0 mL) were stirred at 100° C. for 2 hr, and 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 min. and diluted with ethyl acetate. The resulting byproduct 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).
後処理
- customThe resulting byproduct N-phenylmorpholine-4-carboxamide was removed by filtration
- concentrationThe filtrate was concentrated
- custompurified by silica gel column chromatography (ethyl acetate/hexane→methanol/ethyl acetate)
出典と根拠
- ORDレコード
- ord-bfd77aef3f3c42d79a38c985fbbbe7a3
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08883788B2
反応ノート
読み込み中…