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

HRID 1608762

반응식

HRID 1608762 반응식
[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

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 6336Myclobutanil

생성물 1

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

시약·촉매·용매 1

HCID 14923Ammonium Hydroxide용매

반응 조건

온도
90 °C

실험 절차

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, Example 157 of Table 1.

후처리

  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

출처 및 근거

ORD 기록
ord-e7c45300e6f5489395ed17598005c8ca
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05397768

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