Potassium Cyanide → HCID 178510898、化合物

HRID 436210

反応式

HRID 436210 の反応式
Cl[CH2:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=2)[NH:5][N:4]=1.[C-:13]#[N:14].[K+]>C(O)C.O>[C:13]([CH2:2][C:3]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([Cl:12])[CH:10]=2)[NH:5][N:4]=1)#[N:14]

参加物

5

反応物 2

HCID 9032Potassium CyanideHCID 178478451HCID 178478451、化合物

生成物 1

HCID 178510898HCID 178510898、化合物収率 69.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

A solution of 3-chloromethyl-5-chloro-1H-indazole (4.5 g) in ethanol (50 ml) is dropwise added to a solution of potassium cyanide (17 g) in water (10 ml) while stirring at 5° C, and the resulting mixture is stirred at room temperature for 2 hours and at 50° C for 2 hours. The reaction mixture is cooled and the precipitated potassium chloride is removed by filtration. The filtrate is concentrated under reduced pressure, admixed with water and extracted with ether. The ether layer is washed with water, dried over anhydrous magnesium sulfate and concentrated to give 3-cyanomethyl-5-chloro-1H-indazole (3.0 g) as resinous material.

後処理

  1. stirringthe resulting mixture is stirred at room temperature for 2 hours and at 50° C for 2 hours
  2. temperatureThe reaction mixture is cooled
  3. customthe precipitated potassium chloride is removed by filtration
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. extractionextracted with ether
  6. washThe ether layer is washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-b592167866d14dcd8943918814b4694a
出典データセット
uspto-grants-1977_02
特許番号
US04008070

関連ノート

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