1H-1,2,4-Triazole → 4-(1,2,4-Triazol-1-ylmethyl)benzonitrile

HRID 1111161

반응식

HRID 1111161 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]#[N:10])=[CH:5][CH:4]=1.[NH:11]1[CH:15]=[N:14][CH:13]=[N:12]1>C(Cl)(Cl)Cl.C(#N)C>[CH:8]1[C:3]([CH2:2][N:11]2[N:12]=[CH:13][N:14]=[CH:15]2)=[CH:4][CH:5]=[C:6]([C:9]#[N:10])[CH:7]=1

참가 물질

5

반응물 2

HCID 92571H-1,2,4-TriazoleHCID 869964-(Bromomethyl)benzonitrile

생성물 1

HCID 75376164-(1,2,4-Triazol-1-ylmethyl)benzonitrile

시약·촉매·용매 2

HCID 6212Chloroform용매HCID 6342Acetonitrile용매

실험 절차

A solution containing alpha-bromo-4-tolunitrile (19.6 g) and 1,2,4-triazole (30.5 g) in a mixture of chloroform (250 mL) and acetonitrile (50 mL) is stirred at reflux for 15 hours. The solution is cooled and washed with 3% aqueous sodium bicarbonate (200 mL) and the organic solution is then dried (MgSO4) and evaporated. The residue is chromatographed on silica gel (300 g). Elution with chloroform/isopropanol (10:1) affords 4-[1-(1,2,4-triazolyl)methyl]-benzontrile, m.p. 77°-79°, which forms a hydrochloride salt, m.p. 200°-205°, when its solution in ethyl acetate is treated with ethereal HCl.

후처리

  1. temperatureat reflux for 15 hours
  2. temperatureThe solution is cooled
  3. washwashed with 3% aqueous sodium bicarbonate (200 mL)
  4. dry with materialthe organic solution is then dried (MgSO4)
  5. customevaporated
  6. customThe residue is chromatographed on silica gel (300 g)
  7. washElution with chloroform/isopropanol (10:1)

출처 및 근거

ORD 기록
ord-75608f9dafaa46ef8d42a7355ab039bb
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04978672

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