反应详情

To a solution of 173 mg. (1 m mole) of 3-hydroxy-5-chlorobenzoic acid in 2 ml. of dimethylformamide is added 85 mg. (2 m moles) of 56.6% sodium hydride in an oil suspension. After ten minutes, the resulting suspension is treated with 130 mg. (1 m mole) of benzyl chloride and the mixture heated to 100° C. for one hour. The reaction mixture is then cooled, diluted with 5 ml. of water, and extracted with ether. The aqueous phase is separated, acidified with 6N hydrochloric acid and the product extracted with ether. The ether solvent is removed in vacuo and the residual product triturated with water and filtered. The dried product is sublimed at 125° C. and 0.02 mm of pressure to provide 50 mg. of the desired produce, m.p. 127-129° C.

1. waitAfter ten minutes
2. additionthe resulting suspension is treated with 130 mg
3. temperatureThe reaction mixture is then cooled
4. additiondiluted with 5 ml
5. extractionof water, and extracted with ether
6. customThe aqueous phase is separated
7. extractionthe product extracted with ether
8. customThe ether solvent is removed in vacuo
9. customthe residual product triturated with water
10. filtrationfiltered
11. customis sublimed at 125° C.
12. custom0.02 mm of pressure to provide 50 mg
13. customof the desired produce