反应详情

Nitric acid (69% by weight, 16M, 20 ml) was added dropwise to a solution of methyl (4-hydroxyphenyl)acetate [from step 2] (50.0 g, 0.3 mole) in acetic acid (500 ml), maintaining the temperature of the reaction below 15° C. by external cooling. (An induction period was observed for this reaction.) Once gas chromatographic analysis had confirmed that the reaction was complete, the mixture was carefully quenched into water (21) with vigorous stirring. An emulsion formed which subsequently crystallised. After filtration, washing with water and drying, the desired product was obtained as a yellow powder.

1. temperaturemaintaining
2. customthe temperature of the reaction below 15° C. by external cooling
3. custom(An induction period was observed for this reaction
4. customthe mixture was carefully quenched into water (21) with vigorous stirring
5. customAn emulsion formed which
6. customsubsequently crystallised
7. filtrationAfter filtration
8. washwashing with water
9. customdrying