Fenbuconazole → HCID 15790296、化合物

HRID 1656014ノート

反応式

HRID 1656014 の反応式
[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

参加物

4

反応物 2

HCID 86138FenbuconazoleHCID 21226445Aluminium lithium hydride

生成物 1

HCID 15790296HCID 15790296、化合物収率 89.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-b0097046da0c4cec9ece5ca4a55073c6
出典データセット
uspto-grants-1993_10
特許番号
US05252594

反応ノート

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