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 30 min, and diluted with ethyl acetate. The resulting solid was removed by filtration. The filtrate was concentrated, and the residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate) to give the title compound (9.61 g).
後処理
- customThe resulting solid was removed by filtration
- concentrationThe filtrate was concentrated
- customthe residue was purified by column chromatography (ethyl acetate/hexane-methanol/ethyl acetate)
出典と根拠
- ORDレコード
- ord-431a0c70d78e4904b73982c60d4ce753
- 出典データセット
- uspto-grants-2015_07
- 特許番号
- US09090586B2
反応ノート
読み込み中…