반응 #44442

반응 방정식

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

→

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

수율 98.2%

용매

DMF

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   workup.ADDITIONpoured into water
3. 3
   추출extracted with diethyl ether
4. 4
   세척The organic layer was washed with water
5. 5
   건조dried (Na2SO4)
6. 6
   기타evaporated

실험 절차

10 mg Pd/C 10% was added to a solution of trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (100 mg, 0.25 mmol) in 5 mL of DMF. The suspension was shaken under H2 atmosphere for 2 days. The mixture was filtered, poured into water and extracted with diethyl ether. The organic layer was washed with water, dried (Na2SO4) and evaporated to give trans-N-(2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (89 mg, 98%). Data: 1H-NMR (400 MHz, CDCl3) 1.85 (m, 3H), 2.99 (m, 1H), 3.18 (m, 1H), 3.75 (m, 1H), 4.50 (d, J=8,1H), 4.72 (m, 1H), 6.62 (br, 1H), 6.84-7.30 (8 arH). (m/z)=362 (M+H)+.

출처