HCID 22321559、化合物 → 4-(chloromethyl)-1-methyl-1H-1,2,3-triazole hydrochloride
反応式
O.[ClH:2].[CH3:3][N:4]1[CH:8]=[C:7]([CH2:9]O)[N:6]=[N:5]1>S(Cl)(Cl)=O>[ClH:2].[Cl:2][CH2:9][C:7]1[N:6]=[N:5][N:4]([CH3:3])[CH:8]=1参加物
3
実験手順
To thionyl chloride (20 ml) under nitrogen, cooled by an ice bath, was added (1-methyl-1H-[1,2,3]triazol-4-yl)methanol hydrochloride monohydrate (1.996 g, 11.9 mmol). The mixture was stirred for 5 min before removing the cooling bath and heating at reflux for 30 min. The excess thionyl chloride was evaporated in vacuo and the residue was triturated with diethyl ether. The resulting solid was collected by filtration, washed with diethyl ether and dried under vacuum at 60° C. to give the title compound as a white solid: 1H NMR (360 MHz, DMSO-d6) δ 4.04 (3H, s), 4.81 (2H, s), 8.13 (1H, s).
後処理
- custombefore removing the cooling bath
- temperatureheating
- temperatureat reflux for 30 min
- customThe excess thionyl chloride was evaporated in vacuo
- customthe residue was triturated with diethyl ether
- filtrationThe resulting solid was collected by filtration
- washwashed with diethyl ether
- customdried under vacuum at 60° C.
出典と根拠
- ORDレコード
- ord-2774937715ea49fd92305f4b40213359
- 出典データセット
- uspto-grants-2005_03
- 特許番号
- US06872720B2
反応ノート
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