反応 #674317

反応方程式

NaHCO3

2,4-dichloro-1,3,5-triazine

(3-aminophenyl)-methanesulfonamide

water

→

A1

3-[(4-Chloro-1,3,5-triazin-2-yl)amino]benzenemethanesulfonamide

溶媒

DMF

DMF

反応条件

後処理

1. 1
   抽出The aqueous layer was extracted with EtOAc
2. 2
   乾燥the combined organic layers were dried over Na2SO4
3. 3
   その他Evaporation of solvent

実験手順

To a solution of 2,4-dichloro-1,3,5-triazine (1.0 eq) in dry DMF (0.7 M) at 0° C. under N2 atmosphere was added a solution of (3-aminophenyl)-methanesulfonamide (1.0 eq) in dry DMF (0.7 M). The reaction mixture was stirred for 2.5 h at 0° C. Then water was added and the aqueous solution was neutralized with sat. aq. NaHCO3 solution. The aqueous layer was extracted with EtOAc and the combined organic layers were dried over Na2SO4. Evaporation of solvent gave A1 as a white solid which was used in the next step without further purification. 1H NMR (400 MHz, d6-DMSO, 300K) δ 4.26 (s, 2H), 6.89 (s, 2H), 7.15 (d, J=7.4 Hz, 1H), 7.36 (d, J=7.4 Hz, 1H), 7.66 (d, J=7.4 Hz, 1H), 8.64 (s, 1H), 9.75 (br. s, 1H), 10.83 (s, 1H). MS (ES) C10H10ClN5O2S requires: 299. found: 300 (M+H)+.

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