Ammonia → HCID 66911322, 화합물

HRID 128176

반응식

HRID 128176 반응식
N.[Na].[C:3](#[N:5])[CH3:4].[Cl:6][C:7]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:8]=1[C:9]#[N:10]>O1CCCC1.C(OCC)C>[NH2:10][C:9]([C:8]1[CH:11]=[CH:12][C:13]([Cl:15])=[CH:14][C:7]=1[Cl:6])=[CH:4][C:3]#[N:5]

참가 물질

7

반응물 4

HCID 222Ammonia2회HCID 6342AcetonitrileHCID 810502,4-DichlorobenzonitrileHCID 5360545Sodium2회

생성물 1

HCID 66911322HCID 66911322, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

A 150 ml. portion of ammonia is condensed in a reaction flask and a small piece of sodium is added. The blue color is discharged by the addition of ferric chloride and 3.22 g. of sodium are added. After the color is discharged, 5.75 ml. of acetonitrile in 10 ml. of diethyl ether are added. The reaction is cooled in a dry ice-acetone bath and 16.6 g. of 2,4-dichlorobenzonitrile in 25 ml. of tetrahydrofuran are added dropwise. The ammonia is allowed to evaporate, the solvent is blown off with nitrogen and water is added. The mixture is extracted with methylene chloride. The organic extracts are dried over sodium sulfate and filtered through Magnesol®. The filtrate is evaporated with the addition of hexanes giving β-amino-2,4-dichlorocinnamonitrile as a white crystalline solid.

후처리

  1. customcondensed in a reaction flask
  2. temperatureThe reaction is cooled in a dry ice-acetone bath
  3. customto evaporate
  4. additionis added
  5. extractionThe mixture is extracted with methylene chloride
  6. dry with materialThe organic extracts are dried over sodium sulfate
  7. filtrationfiltered through Magnesol®
  8. customThe filtrate is evaporated with the addition of hexanes

출처 및 근거

ORD 기록
ord-dd048b94224743e08eb1b84638c779d4
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259256

연결된 노트

불러오는 중…