Sodium Cyanide → HCID 12071532、化合物

HRID 1841435ノート

反応式

HRID 1841435 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9]=[N+:10]([O-])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[C-:18]#[N:19].[Na+]>P([O-])(O)(O)=O.[K+].CO.O.C(Cl)Cl>[C:11]1([N:10]=[C:9]([C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([Cl:8])[C:2]=2[Cl:1])[C:18]#[N:19])[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

7

反応物 2

HCID 8929Sodium CyanideHCID 71363014(2,3-Dichlorophenyl)-N-phenylmethanimine N-oxide

生成物 1

HCID 12071532HCID 12071532、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 516951Monobasic potassium phosphate溶媒

反応条件

温度
0 °C

実験手順

635 mMol of N-(2,3-dichlorophenylmethylene)anilin-N-oxide (IX) are dissolved in a 5.61 mixture (1:1) of an aqueous 0.5 molar solution of potassium dihydrogenphosphate and methanol adjusted to pH5. To this are added 65 g (1.3 Mol) of sodium cyanide in 200 ml water at approximately 50° C. During the reaction the pH balance is held constant between 8.0 and 8.5. After the reaction is complete (DC control), the reaction mixture is neutralized and cooled to 0° C. The separated yellow-brown crystals are then dissolved in methylene dichloride. The organic phase is washed in water, dried and evaporated under vacuum. The residue is recrystallized from a small amount of methanol.

後処理

  1. customDuring the reaction the pH balance
  2. washThe organic phase is washed in water
  3. customdried
  4. customevaporated under vacuum
  5. customThe residue is recrystallized from a small amount of methanol

出典と根拠

ORDレコード
ord-02a1b3591a7340ee9eb718fc8e94e344
出典データセット
uspto-grants-2004_01
特許番号
US06683182B2

反応ノート

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