3-Chloro-2,2-dimethylpropanoyl chloride → 3-chloro-N-hydroxy-2,2-dimethylpropanamide

HRID 973951ノート

反応式

HRID 973951 の反応式
Cl.[NH2:2][OH:3].[Cl:4][CH2:5][C:6]([CH3:11])([CH3:10])[C:7](Cl)=[O:8]>O.[OH-].[Na+]>[Cl:4][CH2:5][C:6]([CH3:11])([CH3:10])[C:7]([NH:2][OH:3])=[O:8]

参加物

5

反応物 2

HCID 613453-Chloro-2,2-dimethylpropanoyl chlorideHCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 37127643-chloro-N-hydroxy-2,2-dimethylpropanamide

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 14798Sodium Hydroxide溶媒2 回

実験手順

To a solution of hydroxylamine hydrochloride (50.0 g, 0.7195 mol) in 150 mL of water, 50% aqueous sodium hydroxide solution is added dropwise until a pH of 7.0-7.2 is obtained. The solution is cooled to 20°-25° C. and 3-chloropivaloyl chloride (100.0 g, 0.6426 mol) is added dropwise maintaining a pH of 7.0-7.2 with 50% aqueous sodium hydroxide solution and a reaction pot temperature <30° C. The total addition time is 1 hour. This yellow slurry is stirred at room temperature overnight then diluted with water (200 mL). The hydroxamic acid is extracted with ethyl acetate (2×200 mL) and washed with water (200 mL). The organic layer is dried over magnesium sulfate and concentrated to 46.3 g of the title compound as a yellow solid and used without further purification.

後処理

  1. customis obtained
  2. temperatureThe solution is cooled to 20°-25° C.
  3. customa reaction pot temperature <30° C
  4. additionThe total addition time
  5. extractionThe hydroxamic acid is extracted with ethyl acetate (2×200 mL)
  6. washwashed with water (200 mL)
  7. dry with materialThe organic layer is dried over magnesium sulfate
  8. concentrationconcentrated to 46.3 g of the title compound as a yellow solid
  9. customused without further purification

出典と根拠

ORDレコード
ord-73091171216448c8afa066dae38b8de1
出典データセット
uspto-grants-1991_11
特許番号
US05066665

反応ノート

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