Dichloromethane → HCID 19871100, 화합물

HRID 329595

반응식

HRID 329595 반응식
C(O)(=O)C(O)=O.[CH:7]([NH:10][OH:11])([CH3:9])[CH3:8].[OH-].[Na+].[Br:14][CH:15]([CH2:19]Br)[C:16](Cl)=[O:17].C(Cl)Cl>O>[Br:14][CH:15]1[CH2:19][O:11][N:10]([CH:7]([CH3:9])[CH3:8])[C:16]1=[O:17]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 14798Sodium Hydroxide3회HCID 867902,3-Dibromopropanoyl chlorideHCID 19871111HCID 19871111, 화합물

생성물 1

HCID 19871100HCID 19871100, 화합물수율 63.4%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
0 °C

실험 절차

To a stirred mixture of 6 g (25 mmol) of N-isopropylhydroxylamine oxalate and 1N sodium hydroxide (50 ml) in water (100 ml) cooled to 0° C. there was added 2,3-dibromopropionyl chloride (12.5 g, 50 mmol), followed by the addition of 50 ml of 1N sodium hydroxide. Ten minutes later, 150 ml of methylene chloride and 60 ml of 1N sodium hydroxide were added. The mixture was stirred continuously for one hours following which the organic phase was separated, dried over anhydrous magnesium sulfate and concentrated. The concentrate was chromatographed on silica gel with 40% ethyl acetatehexane to afford 3.3 g of 4-bromo-2-isopropyl-3-isoxazolidinone.

후처리

  1. customwas separated
  2. dry with materialdried over anhydrous magnesium sulfate
  3. concentrationconcentrated
  4. customThe concentrate was chromatographed on silica gel with 40% ethyl acetatehexane

출처 및 근거

ORD 기록
ord-730eb489b9ec4f098361805efb92dc25
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04892870

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