反应详情

The process is performed in the same manner as previously (Example 13), starting with 138 g (1.466 mol; 1.15 eq.) of phenol, 109.5 g (2.738 mol; 2.15 eq.) of NaOH, 530 ml of distilled water and 308.9 g (1.275 mol; 1 eq.) of N-(3-chloropropyl)-N,N-dibutylamine hydrochloride. The mixture is refluxed for 16 hours. The oil formed is separated out by settling and washed with 500 ml of water and then diluted with 500 ml of MTBE and washed with 500 ml of 2% HCl. The MTBE phase is concentrated under vacuum and the oil is dried by azeotropic distillation with DCM. 307.1 g of the crude derivative N,N-dibutyl-N-(3-phenoxypropyl)amine are obtained.

1. temperatureThe mixture is refluxed for 16 hours
2. customThe oil formed
3. customis separated out
4. washwashed with 500 ml of water
5. additiondiluted with 500 ml of MTBE
6. washwashed with 500 ml of 2% HCl
7. concentrationThe MTBE phase is concentrated under vacuum
8. dry with materialthe oil is dried by azeotropic distillation with DCM