反应详情

To a mixture of 50 ml of 12.5% phosgene in benzene and 50 ml of tetrahydrofuran which has been cooled to 0° to +5° is added slowly a mixture of 0.05 mole of ethyl lactyllactate and 0.05 mole of triethylamine in 50 of tetrahydrofuran. The above reaction mixture is stirred at 0° to +5° for 2 hours and is then added dropwise to a mixture of 3 gm of methylhydrazine and 0.05 moles of triethylamine in 50 ml of tetrahydrofuran which has been cooled to 0° to +5°. After stirring for 3 hours the reaction mixture is filtered to remove triethylamine hydrochloride. The filtrate is then concentrated in vacuo to give 13.6 gm of crude product. Chromatography on 700 gm of silica gel and elution with methanol/methylene chloride give 6.9 gm of 2-azaalanyllactyllactic acid ethyl ester.

1. temperaturehas been cooled to 0° to +5°
2. additionis added slowly
3. customThe above reaction mixture
4. temperaturehas been cooled to 0° to +5°
5. stirringAfter stirring for 3 hours the reaction mixture
6. filtrationis filtered
7. customto remove triethylamine hydrochloride
8. concentrationThe filtrate is then concentrated in vacuo
9. customto give 13.6 gm of crude product
10. washChromatography on 700 gm of silica gel and elution with methanol/methylene chloride