反应详情

To a solution of 3,5-dimethylisothiocyanate (200 mg, 1.2 mmol) in dichloromethane and N,N-dimethylformamide (1:1) (5.0 mL) are added 1,2-diamino-3-chloro-pyrazinium mesitylenate (0.59 g, 0.0017 mol) and diisopropylethyl-amine (791 mg, 6.1 mmol). The reaction mixture is stirred for 1 hour. EDCI (93 mg, 5 mmol) is added and the solution stirred for 2 hours at room temperature before being concentrated to dryness. The residue is taken up in water and stirred for 5 minutes and the solid precipitated was filtered, washed with water, dried to get the product as a light brown solid (0.25 g, 75%). TLC: pet ether/ethyl acetate (6/4) Rf—0.4. LCMS (method A): mass found (M+H+, 274.0), Rt (min): 4.47 area % 98.0 (max), 98.47 (254 nm); 1H NMR (400 MHz, DMSO-d6): δ 9.99 (s, 1H), 8.95 (d, J=4.28 Hz, 1H), 7.91 (d, J=4.32 Hz, 1H), 7.28 (s, 2H), 6.58 (s, 1H), 2.24 (s, 6H).

1. stirringthe solution stirred for 2 hours at room temperature
2. concentrationbefore being concentrated to dryness
3. stirringstirred for 5 minutes
4. customthe solid precipitated
5. filtrationwas filtered
6. washwashed with water
7. customdried