反応 #54235

反応方程式

2-hydrazino-5-(2-methylphenyl)-1,3,4-thiadiazole hydrochloride

acetic anhydride

water

→

2-(2-Acetylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole

溶媒

pyridine

反応条件

後処理

1. 1
   抽出extracted three times with methylene chloride
2. 2
   その他The organic layer was evaporated
3. 3
   洗浄plates by eluting with chloroform-methanol (4:1)
4. 4
   その他The resultant product was crystallised from ethyl acetate (0.32 g; 31%) m.p. 165°-6°

実験手順

A solution of 2-hydrazino-5-(2-methylphenyl)-1,3,4-thiadiazole hydrochloride (1.0 g) in a mixture of acetic anhydride (0.5 ml) and pyridine (0.5 ml) was kept at room temperature under nitrogen for 0.5 hr. The solution was poured into water (100 ml) and extracted three times with methylene chloride. The organic layer was evaporated and the residue was fractionated on two 20 × 20 cm, 2 mm thick silica preparative t.l.c. plates by eluting with chloroform-methanol (4:1). The resultant product was crystallised from ethyl acetate (0.32 g; 31%) m.p. 165°-6°. C11H12N4OS requires C, 52.8; H, 5.6; N, 22.4; S, 12.8 Found C, 52.8; H, 5.1; N, 22.8; S, 13.2%

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