Benzyl Chloride → 2-Benzyloxy-6-chlorotoluene
反応式
[Cl:1][C:2]1[C:3]([CH3:9])=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.[CH2:10](Cl)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>C(C(C)=O)C>[CH2:10]([O:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[CH3:9])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1参加物
5
実験手順
A mixture of 143 g (1.0 mol) of 3-chloro-2-methylphenol, 139 g (1.1 mol) of benzyl chloride, 276 g (2.0 mol) of potassium carbonate and 680 g of methyl ethyl ketone (MEK) is heated under reflux with stirring. After 8 hours, a further 25 g (0.18 mol) of potassium carbonate are added and the mixture is then heated under reflux for a further 8 hours. The batch is filtered and the filter cake is washed with MEK. After working up by distillation, 206 g of 2-benzyloxy-6-chlorotoluene (b.p. 161 ° C., 3 mbar) are obtained as a pale yellow liquid in 99.6% purity (surface area % according to GC). This corresponds to a yield of 88.3% of theory.
後処理
- temperatureis heated
- temperatureunder reflux
- temperaturethe mixture is then heated
- temperatureunder reflux for a further 8 hours
- filtrationThe batch is filtered
- washthe filter cake is washed with MEK
- distillationAfter working up by distillation, 206 g of 2-benzyloxy-6-chlorotoluene (b.p. 161 ° C., 3 mbar)
- customare obtained as a pale yellow liquid in 99.6% purity (surface area % according to GC)
出典と根拠
- ORDレコード
- ord-fedab3ab2c1942d7bfcf8c467207f665
- 出典データセット
- uspto-grants-1999_06
- 特許番号
- US05910605
反応ノート
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