Réaction #44444

Équation de réaction

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

Rendement 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

Rendement 96.1%

Solvants

ethanol

Conditions de réaction

Traitement

1. 1
   TempératureAfter cooling the mixture
2. 2
   Autrewas 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
   Filtrationthe mixture was filtered
6. 6
   ExtractionThe filtrate was extracted with ethyl acetate
7. 7
   Lavagethe organic layer was washed with brine
8. 8
   Séchagedried (Na2SO4)
9. 9
   Autreevaporated

Mode opératoire

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)+.

Source