反応 #44458

反応方程式

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

収率 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

収率 48.0%

溶媒

CH2Cl2

反応条件

後処理

1. 1
   その他The reaction mixture was quenched with sat. NaHCO3 (aq)
2. 2
   抽出extracted with CH2Cl2
3. 3
   その他The organic layer was dried
4. 4
   その他evaporated
5. 5
   その他The crude product was purified on silica and by HPLC

実験手順

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)+.

出典