Potassium Hydroxide → Diniconazole

HRID 1902987노트

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HRID 1902987 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[C:10](/[N:31]1[CH:35]=[N:34][CH:33]=[N:32]1)\[CH:11](C(OC1C(C(C)C)CCC(C)C1)C([O-])=O)[C:12]([CH3:15])([CH3:14])[CH3:13].[OH-:36].[K+]>C(O)C>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1/[CH:9]=[C:10](/[N:31]1[CH:35]=[N:34][CH:33]=[N:32]1)\[CH:11]([OH:36])[C:12]([CH3:15])([CH3:14])[CH3:13]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 86739295(+)-[(E)-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-yl]-(-)-menthoxyacetate

생성물 1

HCID 6436605Diniconazole수율 79.9%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
25 °C

실험 절차

A mixture of 1.6 g of (-)-[(E)-1-(2,4-dichlorphenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-yl]-(-)-menthoxyacetate and 30 cc of a 95% aqueous ethanol solution containing 0.2 g of potassium hydroxide was stirred at 25° C. for one hour. The reaction mixture was poured into 200 cc of ice water and extracted with 300 cc of ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting crude crystals were recrystallized from a carbon tetrachloride-n-hexane mixture to obtain 0.8 g of (-)-(E)-1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-4,4-dimethyl-1-penten-3-ol: [α]D24 -31.7 (c=1, CHCl3), melting point 160°-161° C. The NMR spectrum was the same as that of the racemate described in Reference Example 2.

후처리

  1. extractionextracted with 300 cc of ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. concentrationconcentrated in vacuo
  4. customThe resulting crude crystals were recrystallized from a carbon tetrachloride-n-hexane mixture

출처 및 근거

ORD 기록
ord-9858e83f0c584216880b098f526bfafb
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04435203

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