反应详情

温度

-10 °C

Under a nitrogen atmosphere 100 mg (0.227 mmol) 6-[4-(7-methoxy-2-oxo-1,2,4,5-tetrahydro-benzo[d][1,3]diazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylic acidmethoxy-methyl-amide were cooled to −10° C. in 5.00 mL THF and combined with 0.400 mL (0.400 mmol) phenylmagnesium bromide solution (1M in THF). The mixture was stirred for 1 h at −10° C. and then heated to 0° C. Then 0.200 mL (0.200 mmol) phenylmagnesium bromide solution (1M in THF) were added, the mixture was stirred for 1 h and then heated to RT. The reaction mixture was combined with a saturated ammonium chloride solution and extracted with EtOAc. The combined organic phases were dried and evaporated down i. vac. The residue was purified by preparative HPLC-MS. The fractions containing the product were combined and evaporated down by half. The precipitate formed was suction filtered and dried.

1. temperatureheated to 0° C
2. stirringthe mixture was stirred for 1 h
3. temperatureheated to RT
4. extractionextracted with EtOAc
5. customThe combined organic phases were dried
6. customevaporated down i
7. customThe residue was purified by preparative HPLC-MS
8. additionThe fractions containing the product
9. customevaporated down by half
10. customThe precipitate formed
11. filtrationfiltered
12. customdried