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

HRID 727839ノート

反応式

HRID 727839 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒2 回HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f942d85ed94c4f01b99c0feca55ffa61
出典データセット
uspto-grants-1991_09
特許番号
US05045556

反応ノート

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