Methanol → 4,6-Diaminonicotinonitrile

HRID 617924

반응식

HRID 617924 반응식
Br[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([NH2:9])[C:3]=1[C:10]#[N:11].[H][H].C([O-])(=O)C.[K+].CO>[Pd].O1CCCC1>[NH2:8][C:6]1[CH:5]=[C:4]([NH2:9])[C:3]([C:10]#[N:11])=[CH:2][N:7]=1

참가 물질

7

반응물 4

HCID 887MethanolHCID 1706684,6-Diamino-2-bromo-3-pyridinecarbonitrileHCID 517044Potassium AcetateHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 2958964,6-Diaminonicotinonitrile

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 8028Tetrahydrofuran용매

실험 절차

A suspension of 21.3 g of 6-bromo-2,4-diamino-5-cyanopyridine (JACS, 80:2838-2840 (1958)) and 1 g of 20% palladium on charcoal in 250 mL of tetrahydrofuran was shaken in a Parr apparatus under an atmosphere hydrogen. After 2 hours, the reaction was stopped and 10 g of potassium acetate and 50 mL of methanol added. The reaction was recharged with hydrogen and shaken for 18 hours. The solvents were removed under reduced pressure and the residue crystallized from isopropyl alcohol to afford the title compound 2,4-diamino-5-cyanopyridine, mp 201-202° C.

후처리

  1. customThe solvents were removed under reduced pressure
  2. customthe residue crystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-c68c356a278b4eea9c94eb125607496a
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952342

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