反应详情

26.9 g (0.14 mol) of trimethoxypropionic acid ethyl ester (prepared according to DT-OS 2,042,920 ) are dissolved in 100 ml of absolute methanol, 7 ml of glacial acetic acid are added and the mixture is heated to the boil. 23.4 g (0.12 mol) of 3-nitro-2,4,6-trimethylphenylhydrazine (prepared according to DT-OS 2,156,913) are introduced in portions into the mixture over the course of 10 minutes. The mixture is stirred for a further 10 minutes at the boil and is allowed to cool whilst stirring. The orange crystals which have precipitated are filtered off, washed with a little methanol and dried (18 hours in vacuo at 50° C.). 14.4 g of β-methoxy-β-(3-nitro-2,4,6-trimethylphenylhydrazino)-acrylic acid ethyl ester of melting point 82° - 83° C. are obtained.

1. temperaturethe mixture is heated to the boil
2. temperatureto cool
3. stirringwhilst stirring
4. customThe orange crystals which have precipitated
5. filtrationare filtered off
6. washwashed with a little methanol
7. customdried (18 hours in vacuo at 50° C.)