4-Cyanopyridine → Pyridine-4-amidine hydrochloride

HRID 393739

반응식

HRID 393739 반응식
C[O-].[Na+].[C:4]([C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1)#[N:5].[Cl-:12].[NH4+:13]>CO>[ClH:12].[C:4]([NH2:13])(=[NH:5])[C:6]1[CH:11]=[CH:10][N:9]=[CH:8][CH:7]=1

참가 물질

5

반응물 3

HCID 75064-CyanopyridineHCID 25517Ammonium ChlorideHCID 10942334Sodium Methoxide

생성물 1

HCID 2776844Pyridine-4-amidine hydrochloride수율 47.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium methoxide (0.54 g) and 4-cyanopyridine (10.4 g) were combined in anhydrous methanol (100 ml) and stirred at room temperature for 18 h, under a nitrogen atmosphere. Ammonium chloride (5.99 g) was then added, and the mixture heated to reflux for 4 h, under a calcium chloride guard tube. The reaction was cooled, evaporated under reduced pressure, re-suspended in ethanol (120 ml) and heated to reflux for another 15 min. The resultant white precipitate was filtered off, dried, then triturated with ice-cold water and dried under vacuum at 40° C. to yield the title compound as a white solid (7.44 g, 47%). Two further crops were obtained through concentration of the ethanol filtrate (total yield 12.1 g, 77%)

후처리

  1. temperaturethe mixture heated
  2. temperatureto reflux for 4 h, under a calcium chloride guard tube
  3. temperatureThe reaction was cooled
  4. customevaporated under reduced pressure
  5. temperatureheated
  6. temperatureto reflux for another 15 min
  7. filtrationThe resultant white precipitate was filtered off
  8. customdried
  9. customtriturated with ice-cold water
  10. customdried under vacuum at 40° C.

출처 및 근거

ORD 기록
ord-0e21b225ba294f82a2884000b6fecbce
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06809100B2

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