反応 #46362

反応方程式

(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester

2-chloro-6,7-difluoro-3-methylquinoxaline

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title compound

(S)-2-[(6,7-Difluoro-3-methylquinoxaline-2-ylamino)methyl]-piperidine-1-carboxylic acid tert butylester

溶媒

DMF

反応条件

後処理

1. 1
   温度After cooling
2. 2
   その他the reaction solution was partitioned between ethyl acetate and water
3. 3
   洗浄The organic layer was washed with water, saturated brine
4. 4
   その他dried
5. 5
   その他evaporated
6. 6
   その他The residue was chromatographed over silica gel
7. 7
   洗浄eluting with a gradient of 10 to 50% ethyl acetate in hexane

実験手順

(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (1.14 g), and 2-chloro-6,7-difluoro-3-methylquinoxaline Teng et al PCT Int. Appl (2000), WO00/42026A1 20000720 (1.14 g) were dissolved in DMF (2 ml) and heated to 90° C. for 3 days under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with water, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 10 to 50% ethyl acetate in hexane. The title compound was obtained as a pink foam (0.524 g), MH+ 393.

出典