반응 #44458

반응 방정식

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

propionyl chloride

triethylamine

→

title compound

수율 48.0%

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

수율 48.0%

용매

CH2Cl2

반응 조건

후처리

1. 1
   기타The reaction mixture was quenched with sat. NaHCO3 (aq)
2. 2
   추출extracted with CH2Cl2
3. 3
   기타The organic layer was dried
4. 4
   기타evaporated
5. 5
   기타The crude product was purified on silica and by HPLC

실험 절차

To a solution of trans-N-(7-amino-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido-[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (50 mg, 0.13 mmol) in CH2Cl2 (2 mL) was added propionyl chloride (11 μl, 0.13 mmol) and triethylamine (20 μl, 0.14 mmol). The reaction mixture was stirred for 1.5 h at room temperature. The reaction mixture was quenched with sat. NaHCO3 (aq) and extracted with CH2Cl2. The organic layer was dried and evaporated. The crude product was purified on silica and by HPLC to afford the title compound (27 mg, 48%). Data (m/z)=434 (M+H)+.

출처