반응 #80178

반응 방정식

{2-methoxy-5-[methyl-(tetrahydro-pyran-4-yl)-amino]-phenyl}-thiourea

Br2

→

4-methoxy-N7-methyl-N7-(tetrahydro-pyran-4-yl)-benzothiazole-2,7-diamine

용매

chloroform

반응 조건

후처리

1. 1
   온도After 24 hrs of reflux the mixture
2. 2
   농축was concentrated in vacuo
3. 3
   workup.ADDITIONSodium bicarbonate solution was added until the pH was 10
4. 4
   여과the crystals were collected by filtration

실험 절차

0.28 g (0.95 mmol) {2-methoxy-5-[methyl-(tetrahydro-pyran-4-yl)-amino]-phenyl}-thiourea were dissolved in 15 ml chloroform and 0.05 ml (1.0 mmol) Br2 were added slowly at room temperature. After 24 hrs of reflux the mixture was concentrated in vacuo and the residue suspended in water. Sodium bicarbonate solution was added until the pH was 10, and the crystals were collected by filtration. These were subjected to column chromatography (ethyl acetate) to afford 0.41 g (41 (%o) of 4-methoxy-N7-methyl-N7-(tetrahydro-pyran-4-yl)-benzothiazole-2,7-diamine as an off-white solid. ES-MS m/e (%): 294 (M+H+, 100).

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