Acetone → 1-(Isocyanatomethyl)-4-nitrobenzene
反応式
[Cl-].[N+:2]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11]C(O)=O)=[CH:7][CH:6]=1)([O-:4])=[O:3].[N-:15]=[N+]=[N-].[Na+].C[C:20](C)=[O:21]>C(Cl)(Cl)Cl>[N+:2]([C:5]1[CH:6]=[CH:7][C:8]([CH2:11][N:15]=[C:20]=[O:21])=[CH:9][CH:10]=1)([O-:4])=[O:3]参加物
6
反応条件
- 温度
- 0 °C
実験手順
The chloride of 4-nitrophenylacetic acid in solution in dry acetone (7.5 ml) is slowly added to an aqueous solution of 0.75 g (11.5 mmoles) of sodium azide, cooled down to 0° C. Agitation of the medium is maintained for one hour after the addition is completed, at 0-5° C. The reaction medium is then diluted with 30 ml of chloroform, decanted and the organic phase washed with water (20 ml) followed by a saturated solution of sodium chloride (20 ml). After drying over sodium sulphate, the organic solution is filtered and partly concentrated (* 20 ml) under vacuum.
後処理
- temperatureAgitation of the medium is maintained for one hour
- additionafter the addition
- customis completed, at 0-5° C
- customdecanted
- washthe organic phase washed with water (20 ml)
- dry with materialAfter drying over sodium sulphate
- filtrationthe organic solution is filtered
- concentrationpartly concentrated (* 20 ml) under vacuum
出典と根拠
- ORDレコード
- ord-5bde7b34ab444cdc8b8a0738703ffac9
- 出典データセット
- uspto-grants-2006_10
- 特許番号
- US07122535B2
反応ノート
読み込み中…