반응 #44444

반응 방정식

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

수율 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

수율 96.1%

용매

ethanol

반응 조건

후처리

1. 1
   온도After cooling the mixture
2. 2
   기타was 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
   여과the mixture was filtered
6. 6
   추출The filtrate was extracted with ethyl acetate
7. 7
   세척the organic layer was washed with brine
8. 8
   건조dried (Na2SO4)
9. 9
   기타evaporated

실험 절차

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)+.

출처