Ethanol → 2-Amino-3-(5-chlorobenzotriazol-1-yl)-2-methylpropionitrile

HRID 7217

反応式

HRID 7217 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][C:5]2[N:6]([CH2:9]C(=O)C)[N:7]=[N:8][C:4]=2[CH:3]=1.[C-:15]#[N:16].[Na+].[Cl-].[NH4+:19].[CH2:20](O)[CH3:21]>N>[NH2:19][C:20]([CH3:21])([CH2:9][N:6]1[C:5]2[CH:13]=[CH:14][C:2]([Cl:1])=[CH:3][C:4]=2[N:8]=[N:7]1)[C:15]#[N:16]

参加物

6

反応物 4

HCID 702EthanolHCID 8929Sodium CyanideHCID 25517Ammonium ChlorideHCID 220202531-(5-Chlorobenzotriazol-1-yl)-propan-2-one

生成物 1

HCID 220202682-Amino-3-(5-chlorobenzotriazol-1-yl)-2-methylpropionitrile

試薬・触媒・溶媒 1

HCID 222Ammonia溶媒

実験手順

240 mg of 1-(5-chlorobenzotriazol-1-yl)-propan-2-one are dissolved in 4 ml of a 2-molar solution of ammonia in ethanol, then 64 mg of sodium cyanide and 91 mg of ammonium chloride are added and the mixture is stirred over night at room temperature. The reaction mixture is subsequently concentrated by evaporation in a vacuum, dissolved again in ethyl acetate, and washed with water and saturated sodium chloride solution. The organic phase is separated, dried with magnesium sulphate and concentrated by evaporation. 2-amino-3-(5-chlorobenzotriazol-1-yl)-2-methylpropionitrile is thus obtained.

後処理

  1. concentrationThe reaction mixture is subsequently concentrated by evaporation in a vacuum
  2. dissolutiondissolved again in ethyl acetate
  3. washwashed with water and saturated sodium chloride solution
  4. customThe organic phase is separated
  5. dry with materialdried with magnesium sulphate
  6. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-7ed350118fc746a58b79ffe1365ea045
出典データセット
uspto-grants-2006_08
特許番号
US07084280B2

関連ノート

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