反应详情

Dissolve 3′-(4-methoxymethyl-phenyl)-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-carboxylic acid tert-butyl ester (3.72 g, 9.70 mmol) in dichloromethane (25 mL). Add cold trifluoroacetic acid (30 mL, 44.2 g, 388 mmol, 40 eq.). Stir for 1 hr. Partition the crude reaction mixture between aq. 5N NaOH and dichloromethane. Separate the layers (pH aqueous layer=14). Extract the aqueous layer with dichloromethane (2×50 mL). Combine organic layers, dry over anhydrous Na2SO4, filter and concentrate to obtain the title preparation (2.76 g, 100% yield). LC MS (ES): m/z=285.0 [M+H].

1. customPartition the crude
2. customreaction mixture between aq. 5N NaOH and dichloromethane
3. customSeparate the layers (pH aqueous layer=14)
4. extractionExtract the aqueous layer with dichloromethane (2×50 mL)
5. dry with materialCombine organic layers, dry over anhydrous Na2SO4
6. filtrationfilter
7. concentrationconcentrate
8. customto obtain the title
9. custompreparation (2.76 g, 100% yield)