反应详情

A mixture of N-methyl-o-fluorobenzylamine (27.8 g), 3-chloro-1-phenylpropan-1-ol(34.2 g), 2,2,6,6-tetramethylpiperidine (34.4 ml) and acetonitrile (500 ml) was refluxed for 48 h. The mixture was cooled to room temperature, filtered and the solvent removed. The residue was partitioned between chloroform and aqueous sodium bicarbonate. The organic phase was dried and the solvent removed. The residue was disolved in 60°-80° petrol (150 ml) and allowed to crystallise yielding the title compound (32.4 g) which is cyclodehydrohalogenated as in Example 4.

1. temperaturewas refluxed for 48 h
2. filtrationfiltered
3. customthe solvent removed
4. customThe residue was partitioned between chloroform and aqueous sodium bicarbonate
5. customThe organic phase was dried
6. customthe solvent removed
7. customwas disolved in 60°-80°
8. customto crystallise