반응 #44446

반응 방정식

Benzenesulfonyl chloride

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

triethylamine

→

trans-N-(7-chloro-2,3,4,14b-tetrahydro-8-[(phenylsulfonyl)amino]-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide

수율 43.5%

용매

CH2Cl2

반응 조건

후처리

1. 1
   온도After cooling the mixture
2. 2
   기타was evaporated
3. 3
   기타the crude compound was purified by chromatography on silica
4. 4
   세척Elution with toluene/ethyl acetate 1:0→0:1 (gradient)

실험 절차

Benzenesulfonyl chloride (10 μL, 0.08 mmol) was added under N2 to 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 (5.0 mg, 0.01 mmol) in 1 mL of CH2Cl2 and 2 μL (1.1 eq) of triethylamine. The resulting mixture was stirred at 35° C. for 4 h. After cooling the mixture was evaporated and the crude compound was purified by chromatography on silica. Elution with toluene/ethyl acetate 1:0→0:1 (gradient) gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-8-[(phenylsulfonyl)amino]-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (2.4 mg, 32%). Data: (m/z)=552 (M+H)+.

출처