Sodium Cyanide → HCID 12071532, 화합물

HRID 1841435노트

반응식

HRID 1841435 반응식
[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

참가 물질

7

반응물 2

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

생성물 1

HCID 12071532HCID 12071532, 화합물

시약·촉매·용매 4

HCID 887Methanol용매HCID 962Water용매HCID 6344Dichloromethane용매HCID 516951Monobasic potassium phosphate용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-02a1b3591a7340ee9eb718fc8e94e344
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683182B2

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