Water → 5-(2,6-difluorobenzyl)-4-methyl-4H-1,2,4-triazole-3-carboxamide

HRID 727839노트

반응식

HRID 727839 반응식
[F:1][C:2]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:3]=1[CH2:4][C:5]1[N:6]([CH3:12])[C:7]([CH2:10][OH:11])=[N:8][N:9]=1.O.[C-]#[N:20].[Na+]>C1(C)C=CC=CC=1.[O-2].[O-2].[Mn+4]>[F:17][C:13]1[CH:14]=[CH:15][CH:16]=[C:2]([F:1])[C:3]=1[CH2:4][C:5]1[N:6]([CH3:12])[C:7]([C:10]([NH2:20])=[O:11])=[N:8][N:9]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 8929Sodium CyanideHCID 199042335-(2,6-difluorobenzyl)-3-hydroxymethyl-4-methyl-4H-1,2,4-triazole

생성물 1

HCID 199042355-(2,6-difluorobenzyl)-4-methyl-4H-1,2,4-triazole-3-carboxamide

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매2회HCID 1140Toluene용매

실험 절차

1.43 g (6 mmol) of 5-(2,6-difluorobenzyl)-3-hydroxymethyl-4-methyl-4H-1,2,4-triazole and 5.22 g (60 mmol) of manganese dioxide are heated under reflux in 40 ml of toluene for 3 hours using a water separator. The reaction mixture is then cooled and filtered over Hyflo, and the filtrate is concentrated by evaporation. The residue is added to 90 ml of isopropanol saturated with ammonia. At 0°, 1.47 g (30 mmol) of sodium cyanide and 10.44 g (120 mmol) of manganese dioxide are added. The reaction mixture is stirred for 4 hours at 0° and filtered over Hyflo. The filtrate is concentrated by evaporation. Recrystallisation of the residue from ethanol yields the pure 5-(2,6-difluorobenzyl)-4-methyl-4H-1,2,4-triazole-3-carboxamide.

후처리

  1. temperatureThe reaction mixture is then cooled
  2. filtrationfiltered over Hyflo
  3. concentrationthe filtrate is concentrated by evaporation
  4. additionThe residue is added to 90 ml of isopropanol saturated with ammonia
  5. filtrationfiltered over Hyflo
  6. concentrationThe filtrate is concentrated by evaporation
  7. customRecrystallisation of the residue from ethanol

출처 및 근거

ORD 기록
ord-f942d85ed94c4f01b99c0feca55ffa61
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05045556

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