反应详情

温度

60 °C

A solution of N-{(1R,3S,4S)-2-[2-Amino-5-(3-fluoro-phenyl)-thiazole-4-carbonyl]-2-aza-bicyclo[2.2.1]hept-3-ylmethyl}-2,2,2-trifluoro-acetamide (0.98 mmol) in MeOH (3.2 mL) is treated with a sat. aq. K2CO3 solution (0.3 mL) and stirred at 60° C. for 6 h. After stirring at rt for additional 14 h the mixture is concentrated in vacuo and the residue is made basic by addition of aq. NaOH solution. A 1:1 mixture of TBME and EtOAc is added and the mixture is stirred vigorously for 1 h. The layers are separated and the aq. layer is extracted with a 1:1 mixture of TBME and EtOAc. The combined organic layers are dried over Na2SO4 and concentrated in vacuo to give the desired product which is used without further purification. LC-MS (basic): tR=0.68 min; [M+H]+=347.1.

1. stirringAfter stirring at rt for additional 14 h the mixture
2. concentrationis concentrated in vacuo
3. additionthe residue is made basic by addition of aq. NaOH solution
4. additionA 1:1 mixture of TBME and EtOAc
5. additionis added
6. stirringthe mixture is stirred vigorously for 1 h
7. customThe layers are separated
8. extractionthe aq. layer is extracted with a 1:1 mixture of TBME and EtOAc
9. dry with materialThe combined organic layers are dried over Na2SO4
10. concentrationconcentrated in vacuo