반응 #44443

반응 방정식

Nitric acid

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-(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

수율 93.5%

용매

CH2Cl2

반응 조건

후처리

1. 1
   추출was extracted with ethyl acetate
2. 2
   세척the organic layer was washed with 5% aq. sodium bicarbonate
3. 3
   건조dried (Na2SO4)
4. 4
   기타evaporated

실험 절차

Nitric acid (50 μL, 1.10 mmol) was added at 0° C. to a suspension 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 (210 mg, 0.53 mmol) in 4 mL of CH2Cl2. After stirring the mixture was extracted with ethyl acetate and the organic layer was washed with 5% aq. sodium bicarbonate, dried (Na2SO4) and evaporated to give 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 (219 mg, 90%). Data: 1H-NMR (400 MHz, DMSO) 1.64-1.94 (m, 3H), 2.05 (br, 1H), 3.26 (t, J=8.0, 1H), 4.20 (d, J=8.0, 1H), 4.35 (d, J=8.0, 1H), 4.60 (dq, J=8.0, 3.0, 1H) 7.15 (m, 1H), 7.11-9.21 (6 ArH). (m/z)=443 (M+H)+.

출처