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

HRID 1111161

反応式

HRID 1111161 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-75608f9dafaa46ef8d42a7355ab039bb
出典データセット
uspto-grants-1990_12
特許番号
US04978672

関連ノート

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