Pyridine → HCID 18365510、化合物
反応式
[CH:1]1[CH:6]=[CH:5][C:4]([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[CH:9]=2)=[CH:3][CH:2]=1.N1C=CC=CC=1.[Cl:21][C:22](Cl)([O:24]C(=O)OC(Cl)(Cl)Cl)Cl>C(Cl)Cl>[Cl:14][C:10]1[CH:9]=[C:8]([N:7]([C:4]2[CH:3]=[CH:2][CH:1]=[CH:6][CH:5]=2)[C:22]([Cl:21])=[O:24])[CH:13]=[CH:12][CH:11]=1参加物
5
実験手順
To a solution of 3-chlorodiphenylamine (3.0 g) and pyridine (1.43 mL) in CH2Cl2 (30 mL) was added triphosgene (1.75 g) at 5° C. After stirring at room temperature for 6 hours, the mixture was evaporated, diluted with EtOAc, washed with water and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (hexane-EtOAc 15:1) to give N-(3-chlorophenyl)-N-phenylcarbamoyl chloride (4.05 g) as an oil.
後処理
- customthe mixture was evaporated
- additiondiluted with EtOAc
- washwashed with water and brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by silica gel column chromatography (hexane-EtOAc 15:1)
出典と根拠
- ORDレコード
- ord-a9e957e95e7f41caac5463b50284bc99
- 出典データセット
- uspto-grants-2001_10
- 特許番号
- US06303649B1
反応ノート
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