Thionyl Chloride → 3-(chloromethyl)-4-methyl-4H-1,2,4-triazole hydrochloride
反応式
S(Cl)([Cl:3])=O.O[CH2:6][C:7]1[N:11]([CH3:12])[CH:10]=[N:9][N:8]=1>>[ClH:3].[Cl:3][CH2:6][C:7]1[N:11]([CH3:12])[CH:10]=[N:9][N:8]=1参加物
3
実験手順
To thionyl chloride (2.0 ml) was added at 0° C. 3-hydroxymethyl-4-methyl-4H-1,2,4-triazole (0.15 g), and the mixture was refluxed for 1.5 hour. The reaction mixture was concentrated under reduced pressure, to which was added diethyl ether. Resulting crystals were collected by filtration and dissolved in ethanol, to which was added diethyl ether for recrystallization to afford 3-chloromethyl-4-methyl-4H-1,2,4-triazole hydrochloride (0.22 g) as colorless prisms, m.p. 96°-97° C.
後処理
- concentrationThe reaction mixture was concentrated under reduced pressure, to which
- additionwas added diethyl ether
- customResulting crystals
- filtrationwere collected by filtration
- dissolutiondissolved in ethanol, to which
- additionwas added diethyl ether
- customfor recrystallization
出典と根拠
- ORDレコード
- ord-a3b94bad97f84c95a707606a77dcd282
- 出典データセット
- uspto-grants-1995_04
- 特許番号
- US05405861
反応ノート
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