反应详情

温度

140 °C

0.65 g (4.70 mmol) 3,4-diamino-5-methylphenol were placed in a little methanol and 0.94 mL (10.00 mmol) 3-methoxypropionic acid was added. First the methanol was distilled off and then the mixture was stirred for 2 h at 140° C. The reaction mixture was taken up in DMF/MeOH and purified by chromatography. The fractions containing product were combined and evaporated down i.vac. to leave the aqueous residue. This was neutralised with an aqueous 4M NaOH solution and extracted with ethyl acetate. The organic phase was dried and evaporated down i.vac. and dried.

1. additionwas added
2. distillationFirst the methanol was distilled off
3. custompurified by chromatography
4. additionThe fractions containing product
5. customevaporated down i.vac
6. customto leave the aqueous residue
7. extractionextracted with ethyl acetate
8. customThe organic phase was dried
9. customevaporated down i.vac
10. customand dried