反応 #517751

反応方程式

N4-(2-methylpropyl)quinoline-3,4-diamine

carbon disulfide

ethanol

→

thiazolo[4,5-c]quinoline-2-thiol

溶媒

sodium hydroxide

反応条件

後処理

1. 1
   温度heated
2. 2
   温度at reflux on a steam bath for 2 hours
3. 3
   その他The resulting precipitate was isolated by filtration
4. 4
   洗浄washed with ethanol
5. 5
   その他air dried
6. 6
   その他to provide 4.4 g of crude product
7. 7
   その他reprecipitated with acetic acid
8. 8
   その他The precipitate was isolated by filtration while still hot,
9. 9
   洗浄washed with hexane
10. 10
    その他air dried

実験手順

N4-(2-methylpropyl)quinoline-3,4-diamine (5.4 g, 25 mmol) was combined with carbon disulfide (9 mL, 150 mmol) and ethanol (55 mL) and then heated at reflux on a steam bath for 2 hours. The resulting precipitate was isolated by filtration, washed with ethanol and then air dried to provide 4.4 g of crude product. A portion (1 g) was dissolved in hot dilute sodium hydroxide and then reprecipitated with acetic acid. The precipitate was isolated by filtration while still hot, washed with hexane and then air dried to provide thiazolo[4,5-c]quinoline-2-thiol as a solid, m.p. 282-284° C. Analysis: Calculated for C10H6N2S2: % C, 55.02; % H, 2.77; % N, 12.83: Found: % C, 54.96; % H, 2.69; % N, 12.74.

出典