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ammonia

6-Bromo-4′-methylspiro[chroman-4,2′-imidazole]-5′(1′H)-thione

Intermediate 3

6-Bromo-4′-methylspiro[chroman-4,2′-imidazole]-5′(1′H)-thione

→

title compound

수율 77.0%

6-Bromo-5′-methylspiro[chroman-4,2′-imidazol]-4′-amine

수율 77.0%

용매

MeOH

MeOH

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후처리

1. 1
   기타The solution was evaporated in vacuo
2. 2
   기타Evaporation in vacuo

실험 절차

6-Bromo-4′-methylspiro[chroman-4,2′-imidazole]-5′(1′H)-thione (0.10 g, 0.32 mmol, Intermediate 3) was dissolved in MeOH (1 mL) and 7M ammonia in MeOH (4 mL, 28 mmol) was added. The solution was heated at 60° C. for 12 h in a sealed vial. The solution was evaporated in vacuo. The treatment with 7M ammonia was repeated in the same way one more time. Evaporation in vacuo gave the title compound (73 mg, 77% yield) which was used without further purification in the following step. 1H NMR (400 MHz, CDCl3) δ ppm 2.11 (m, 2 H), 2.35 (s, 3 H), 4.53 (m, 2 H), 4.98 (br s, 2 H), 6.66 (m, 1 H), 6.78 (d, 1 H), 7.22 (m, 1 H); MS (ES+) m/z 294 [M+H]+.

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