Thionyl Chloride → 3-(chloromethyl)-4-methyl-4H-1,2,4-triazole hydrochloride

반응식

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

참가 물질

반응물 2

HCID 24386Thionyl Chloride

HCID 15707893(4-methyl-4H-1,2,4-triazol-3-yl)methanol

생성물 1

HCID 223819093-(chloromethyl)-4-methyl-4H-1,2,4-triazole hydrochloride

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록: ord-a3b94bad97f84c95a707606a77dcd282
출처 데이터셋: uspto-grants-1995_04
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US05405861

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