Sulfuric Acid → 2-(4-Chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]hexanamide

HRID 54903

反応式

HRID 54903 の反応式
[CH2:1]([C:5]([C:14]1[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=1)([CH2:8][N:9]1[CH:13]=[N:12][CH:11]=[N:10]1)[C:6]#[N:7])[CH2:2][CH2:3][CH3:4].S(=O)(=O)(O)[OH:22]>[OH-].[NH4+]>[Cl:20][C:17]1[CH:16]=[CH:15][C:14]([C:5]([CH2:8][N:9]2[CH:13]=[N:12][CH:11]=[N:10]2)([CH2:1][CH2:2][CH2:3][CH3:4])[C:6]([NH2:7])=[O:22])=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 6336Myclobutanil

生成物 1

HCID 199569562-(4-Chlorophenyl)-2-[(1,2,4-triazol-1-yl)methyl]hexanamide収率 56.5%

試薬・触媒・溶媒 1

HCID 14923Ammonium Hydroxide溶媒

反応条件

温度
90 °C

実験手順

To a 500 mL flask was charged 75.0 g (0.24 mole) of alpha-n-butyl-alpha-(4-chlorophenyl)-1H-1,2,4-triazole-1-propanenitrile followed by 300 mL of 95% sulfuric acid. The mixture was stirred at 90° C. for 7 days after which the mixture was cooled to room temperature, diluted with ice and neutralized with ammonium hydroxide until basic (pH 8). The product was extracted with ethylene dichloride then washed with water and dried over magnesium sulfate. The solvent was concentrated and gave 45 g (56.5% yield) of a solid melting point 197°-199° C.

後処理

  1. temperaturewas cooled to room temperature
  2. extractionThe product was extracted with ethylene dichloride
  3. washthen washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationThe solvent was concentrated

出典と根拠

ORDレコード
ord-ca88297e1e8d45faa969928145c45ee2
出典データセット
uspto-grants-1997_04
特許番号
US05624916

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