Benzoyl Peroxide → Propanedioic acid, (2-bromo-1-methylethylidene)-, diethyl ester

HRID 1517196노트

반응식

HRID 1517196 반응식
[C:1](=[C:4]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6])([CH3:3])[CH3:2].[Br:15]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:15][CH2:3][C:1](=[C:4]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH3:2]

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimide2회HCID 81255Diethyl isopropylidenemalonate

생성물 1

HCID 11254458Propanedioic acid, (2-bromo-1-methylethylidene)-, diethyl ester

시약·촉매·용매 1

HCID 5943Carbon Tetrachloride용매2회

실험 절차

Diethyl isopropylidenemalonate (4, 50g, 0.25 mol) was refluxed with stirring with N-bromosuccinimide (44.3 g, 0.25 mol) and dibenzoyl peroxide (1.0 g, 4.1 mmol) in carbon tetrachloride (100 mL) with illumination using Kodak Ectagraphic slide projector lamp ELH (300 Watt) for 1.5 h. The reaction was completed as indicated by a negative starch-iodine test for N-bromosuccinimide. The resulting mixture was diluted with carbon tetrachloride (100 mL) and it was cooled in an ice-bath. The precipitated succinimide was filtered off and the filtrate was evaporated in vacuo at room temperature. The residual pale yellow oil of diethyl bromo-isopropylidene-malonate (5, 71.1 g) was used without purification in the Example 2.

후처리

  1. customfor 1.5 h
  2. temperaturewas cooled in an ice-bath
  3. filtrationThe precipitated succinimide was filtered off
  4. customthe filtrate was evaporated in vacuo at room temperature
  5. customThe residual pale yellow oil of diethyl bromo-isopropylidene-malonate (5, 71.1 g) was used without purification in the Example 2

출처 및 근거

ORD 기록
ord-d55ac5bb53bc4f0caf556f10c006cee1
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08232275B2

반응 노트

불러오는 중…