Thionyl Chloride → 3-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride

反応式

O[CH2:2][C:3]1[N:7]([CH2:8][CH2:9][CH3:10])[CH:6]=[N:5][N:4]=1.S(Cl)([Cl:13])=O>>[ClH:13].[Cl:13][CH2:2][C:3]1[N:7]([CH2:8][CH2:9][CH3:10])[CH:6]=[N:5][N:4]=1

参加物

反応物 2

HCID 24386Thionyl Chloride

HCID 229386294-Propyl-4H-1,2,4-triazole-3-methanol

生成物 1

HCID 229387553-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride

実験手順

To 3-hydroxymethyl-4-propyl-4H-1,2,4-triazole (5.95 g), thionyl chloride (40 ml) was slowly added at 0° C. The mixture was heated to reflux for 1 hour, and concentrated under reduced pressure. To the residue was added ethanol, and the mixutre was further concentrated. To the residue were added ethyl acetate and small amount of ethanol, and the precipitated crystals were collected by filtration. The crystals were washed with ethyl acetate, to give 3-chloromethyl-4-propyl-4H-1,2,4-triazole hydrochloride (5.43 g) as pale yellow crystals.

後処理

temperatureThe mixture was heated
temperatureto reflux for 1 hour
concentrationconcentrated under reduced pressure
additionTo the residue was added ethanol
concentrationthe mixutre was further concentrated
additionTo the residue were added ethyl acetate and small amount of ethanol
filtrationthe precipitated crystals were collected by filtration
washThe crystals were washed with ethyl acetate

出典と根拠

ORDレコード: ord-0b0d97d4c55d4af59975b87bece5e632
出典データセット: uspto-grants-2007_08
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07262185B2

反応ノート

読み込み中…

参加物