Sodium Hydroxide → HCID 19871116、化合物

HRID 329596

反応式

HRID 329596 の反応式
Cl.[CH:2]([NH:5][OH:6])([CH3:4])[CH3:3].[OH-].[Na+].[Br:9][CH:10]([CH2:14][CH2:15]Br)[C:11](Cl)=[O:12]>C(Cl)Cl.O>[Br:9][CH:10]1[CH2:14][CH2:15][O:6][N:5]([CH:2]([CH3:4])[CH3:3])[C:11]1=[O:12]

参加物

6

反応物 3

HCID 14798Sodium Hydroxide2 回HCID 170873N-Isopropylhydroxylamine HydrochlorideHCID 44131432,4-Dibromobutyryl chloride

生成物 1

HCID 19871116HCID 19871116、化合物収率 10.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
5 °C

実験手順

To a stirred mixture of 5.3 g (47 mmol) of N-isopropylhydroxylamine hydrochloride in 100 ml of methylene chloride cooled to 5° C. was added 3.8 g (47 mmol) of 50% sodium hydroxide solution in 20 ml of water. To this mixture was added with stirring 12.4 g (47 mmol) of 2,4-dibromobutyrylchloride and twenty minutes later an additional 7.6 g (94 mmol) of 50% sodium hydroxide solution was added. After twenty hours the organic phase was separated, dried over anhydrous magnesium sulfate and concentrated to an oil. This oil was chromatographed on silica gel with 40% ethyl acetate-hexane to afford 1.1 g of oily dihydro-4-bromo-2-isopropyl-2H-1,2-oxazin-3(4H)-one.

後処理

  1. additionTo this mixture was added
  2. additionwas added
  3. customAfter twenty hours the organic phase was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated to an oil
  6. customThis oil was chromatographed on silica gel with 40% ethyl acetate-hexane

出典と根拠

ORDレコード
ord-8993049324244e9cab065f317b7a26b4
出典データセット
uspto-grants-1990_01
特許番号
US04892870

関連ノート

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