Hydrochloric Acid → Triadimenol

HRID 903899

反応式

HRID 903899 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[C:8](=[O:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.[BH4-].[Na+].Cl.C(=O)(O)[O-].[Na+]>CO.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][CH:7]([N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH:8]([OH:13])[C:9]([CH3:11])([CH3:12])[CH3:10])=[CH:19][CH:20]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 39385TriadimefonHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydride

生成物 1

HCID 41368Triadimenol収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
10 °C

実験手順

587 g (2 mols) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-one were dissolved in 3 liters of methanol. A total of 80 g (2 mols) of sodium borohydride was added, in portions of 5 g each, to this solution at 0° to 10° C., while stirring and cooling with ice, and the mixture was stirred at 5° to 10° C. for 2 hours and then at room temperature for 12 hours. It was then cooled to 10° C. and 300 g (3 mols) of concentrated aqueous hydrochloric acid were added at 10° to 20° C. After stirring at room temperature for six hours, the resulting suspension was diluted with 3.8 liters of water which contained 400 g (4.8 mols) of sodium bicarbonate. The precipitate thereby formed was filtered off. 502 g (85% of theory) of 1-(4-chlorophenoxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol of melting point 112°-117° C. were obtained. ##STR12##

後処理

  1. temperaturecooling with ice
  2. stirringthe mixture was stirred at 5° to 10° C. for 2 hours
  3. stirringAfter stirring at room temperature for six hours
  4. customThe precipitate thereby formed
  5. filtrationwas filtered off

出典と根拠

ORDレコード
ord-00a6be36561849159a96b4c8da338168
出典データセット
uspto-grants-1980_10
特許番号
US04229459

関連ノート

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