Sodium Hydroxide → HCID 19871116, 화합물

HRID 329596

반응식

HRID 329596 반응식
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]

참가 물질

6

반응물 3

HCID 14798Sodium Hydroxide2회HCID 170873N-Isopropylhydroxylamine HydrochlorideHCID 44131432,4-Dibromobutyryl chloride

생성물 1

HCID 19871116HCID 19871116, 화합물수율 10.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

반응 조건

온도
5 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8993049324244e9cab065f317b7a26b4
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892870

연결된 노트

불러오는 중…