反应详情

温度

60 °C

Intermediate D2 (13.6 g; 0.0340 mol), 2-hydrazinylacetic acid ethyl ester, hydrochloride (1:1) (10.5 g; 0.0680 mol), N-ethyl-N-(1-methylethyl)-2-propanamine (13.2 g; 0.1020 mol) and t-BuOH (400 ml) were refluxed for 2 hours. The reaction mixture was then evaporated. Water was added and the product was extracted with CH2Cl2. The organic layer was dried on MgSO4, filtered and evaporated in vacuo. The residue was then heated to 60° C. in ethanol/HCl for 1 hour. The reaction mixture was partly evaporated and, the precipitate was filtered off and dried. Yield: 4.57 g of intermediate D3.

1. customThe reaction mixture was then evaporated
2. additionWater was added
3. extractionthe product was extracted with CH2Cl2
4. customThe organic layer was dried on MgSO4
5. filtrationfiltered
6. customevaporated in vacuo
7. customThe reaction mixture was partly evaporated
8. filtrationthe precipitate was filtered off
9. customdried