Ammonia → 3,5-Dimethylpyridine-2,6-diamine

HRID 661017노트

반응식

HRID 661017 반응식
[CH3:1][CH:2]([CH2:5][CH:6]([CH3:9])[C:7]#[N:8])[C:3]#[N:4].[NH3:10]>>[NH2:4][C:3]1[C:2]([CH3:1])=[CH:5][C:6]([CH3:9])=[C:7]([NH2:10])[N:8]=1

참가 물질

3

반응물 2

HCID 222AmmoniaHCID 226729902,4-Dimethylpentanedinitrile

생성물 1

HCID 230493943,5-Dimethylpyridine-2,6-diamine

반응 조건

온도
200 °C

실험 절차

3,5-dimethylglutarimidine is prepared from 2,4-dimethylglutaronitrile using the procedure of Example 2. One equivalent of 3,5-dimethyiglutarimidine is combined with Pd·C catalyst in a Hastelloy shaker tube to which liquid NH3 (59 eq.) is added. The mixture is heated at 200° C. for 45 h. The mixture is cooled to ambient temperature and the excess NH3 removed by N2 purge. The crude mixture is suspended in anhydrous MeOH, the catalyst is removed by syringe filtration, and the crude reaction mixture is concentrated in vacuo. 3,5-dimethylglutarimidine conversion is >90% to give 2,6-diamino-3,5-dimethylpyridine in at least 1% net yield.

후처리

  1. additionis added
  2. temperatureThe mixture is cooled to ambient temperature
  3. customthe excess NH3 removed by N2
  4. custompurge
  5. customthe catalyst is removed by syringe
  6. filtrationfiltration
  7. customthe crude reaction mixture
  8. concentrationis concentrated in vacuo

출처 및 근거

ORD 기록
ord-36a4b2fd7f4c479888e3c255122aa8c8
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084569B2

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