反应 #44444

反应方程式

HCl

SnCl2.2H2O

trans-N-(7-chloro-8-nitro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide

→

title compound

收率 96.1%

trans-N-(8-Amino-7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide

收率 96.1%

溶剂

ethanol

反应条件

后处理

1. 1
   温度After cooling the mixture
2. 2
   其他was evaporated
3. 3
   workup.DISSOLUTIONdissolved in ethyl acetate
4. 4
   workup.ADDITIONAq. sodium bicarbonate was added to the solution (Sn salts were formed)
5. 5
   过滤the mixture was filtered
6. 6
   萃取The filtrate was extracted with ethyl acetate
7. 7
   洗涤the organic layer was washed with brine
8. 8
   干燥dried (Na2SO4)
9. 9
   其他evaporated

实验过程

80 μL 36% HCl and SnCl2.2H2O (600 mg, 2.66 mmol) were added trans-N-(7-chloro-8-nitro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (215 mg, 0.49 mmol) in 10 mL of ethanol. The resulting mixture was stirred at 60° C. for 18 h. After cooling the mixture was evaporated and dissolved in ethyl acetate. Aq. sodium bicarbonate was added to the solution (Sn salts were formed) followed by decalite and the mixture was filtered. The filtrate was extracted with ethyl acetate and the organic layer was washed with brine, dried (Na2SO4) and evaporated to give the title compound (194 mg, 82%). Data: (m/z)=413 (M+H)+.

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