Fenbuconazole → HCID 15790296, 화합물

HRID 2379733노트

반응식

HRID 2379733 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)([CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[C:17]#[N:18])=[CH:10][CH:9]=1>O1CCCC1>[Cl:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)([CH2:19][N:20]2[CH:24]=[N:23][CH:22]=[N:21]2)[CH2:17][NH2:18])=[CH:10][CH:9]=1

참가 물질

4

반응물 2

HCID 86138FenbuconazoleHCID 21226445Aluminium lithium hydride

생성물 1

HCID 15790296HCID 15790296, 화합물수율 89.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A slurry of 18 g (0.45 mole) of lithium aluminum hydride in 1000 mL of dry tetrahydrofuran was cooled to 5° C. while stirring under nitrogen. To the slurry was added alpha-(2-(4-chlorophenyl)ethyl)-alpha-phenyl-1H-1,2,4-triazole-1-propanenitrile in 2000 mL of dry., tetrahydrofuran over 3 hours. The reaction was kept at 5°-10° C. during the addition then allowed to warm to room temperature and stirred overnight. The reaction was cooled in an ice bath and quenched with the slow addition of sodium sulfate. The solvent was removed and the residue was extracted with ethyl acetate and washed with 1000 mL water and 1000 mL brine. After drying, and removal of the solvent, 137 g (89.5% yield) of a very viscous oil resulted.

후처리

  1. customof dry
  2. additionThe reaction was kept at 5°-10° C. during the addition
  3. stirringstirred overnight
  4. temperatureThe reaction was cooled in an ice bath
  5. customquenched with the slow addition of sodium sulfate
  6. customThe solvent was removed
  7. extractionthe residue was extracted with ethyl acetate
  8. washwashed with 1000 mL water and 1000 mL brine
  9. customAfter drying
  10. customremoval of the solvent, 137 g (89.5% yield) of a very viscous oil
  11. customresulted

출처 및 근거

ORD 기록
ord-56dffdbca1ca49edb5650192d421188e
출처 데이터셋
uspto-grants-1994_11
특허 번호
US05364870

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