反応 #54236

反応方程式

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

sodium

methyl iodide

→

2-(2-acetyl-2-methylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole

収率 68.7%

溶媒

ethanol

反応条件

後処理

1. 1
   その他kept at room temperature for 31
2. 2
   その他2 hours
3. 3
   その他The solvent was removed in vacuo
4. 4
   その他the residue chromatographed on a silica column (315 g)
5. 5
   洗浄finally eluting with 5% methanolchloroform
6. 6
   その他The resultant product was crystallised from ethyl acetate

実験手順

2-(2-Acetylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole (6.30 g) was added to a stirred solution of sodium (0.57 g) in ethanol (63 ml) at room temperature. After 15 minutes methyl iodide (7.10 g) was added and the solution kept at room temperature for 31/2 hours. The solvent was removed in vacuo and the residue chromatographed on a silica column (315 g) using mixtures of methanol and chloroform, finally eluting with 5% methanolchloroform. The resultant product was crystallised from ethyl acetate to give 2-(2-acetyl-2-methylhydrazino)-5-(2-methylphenyl)-1,3,4-thiadiazole (4.57 g) m.p. 106°-8°.

出典