反应 #657340

反应方程式

[3-(4-{7-[2-(3-fluoro-phenyl)-ethyl]-2-oxo-2,9-dihydro-10-oxa-1,3,9-triaza-anthracen-3-yl}-piperidin-1-yl)-propyl]-carbamic acid tert-butyl ester

trifluoroacetic acid

→

desired product

收率 99.0%

3-[1-(3-Amino-propyl)-piperidin-4-yl]-7-[2-(3-fluoro-phenyl)-ethyl]-3H,9H-10-oxa-1,3,9-triaza-anthracen-2-one

收率 99.0%

溶剂

dichloromethane

反应条件

后处理

1. 1
   浓缩then concentrated
2. 2
   workup.DISSOLUTIONThe residue was dissolved in water (10 mL)
3. 3
   workup.ADDITIONthen treated with 1.0 N aqueous hydrochloric acid (2.0 mL)
4. 4
   浓缩The resulting solution was concentrated
5. 5
   workup.DISSOLUTIONthe residue was re-dissolved in water (10 mL)
6. 6
   workup.ADDITIONtreated with hydrochloric acid (2.0 mL)
7. 7
   浓缩concentrated
8. 8
   workup.DISSOLUTIONThe residue was dissolved in water (10 mL)
9. 9
   温度the resulting solution was frozen

实验过程

To a solution of [3-(4-{7-[2-(3-fluoro-phenyl)-ethyl]-2-oxo-2,9-dihydro-10-oxa-1,3,9-triaza-anthracen-3-yl}-piperidin-1-yl)-propyl]-carbamic acid tert-butyl ester (94 mg, 0.167 mmol, 1 equiv) in dichloromethane (10 mL) at 23° C. was added trifluoroacetic acid (4.0 mL). The reaction was stirred for 30 min then concentrated. The residue was dissolved in water (10 mL) then treated with 1.0 N aqueous hydrochloric acid (2.0 mL). The resulting solution was concentrated, and then the residue was re-dissolved in water (10 mL), treated with hydrochloric acid (2.0 mL) and concentrated. The residue was dissolved in water (10 mL) and then the resulting solution was frozen and then lyophilized to give 88 mg (0.165 mmol, 99%) of the desired product (dihydrochloride salt) as a yellow solid. LCMS (EI): 464.1 (M+H)+.

来源