m-Chloroperbenzoic acid → 2-[2-(oxiran-2-yl)ethyl]-2,3-dihydro-1H-isoindole-1,3-dione

HRID 1070755

반응식

HRID 1070755 반응식
[CH2:1]([N:5]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:15])[CH2:2][CH:3]=[CH2:4].ClC1C=C(C=CC=1)C(OO)=[O:21].C([O-])(O)=O.[Na+]>ClCCl>[O:21]1[CH2:4][CH:3]1[CH2:2][CH2:1][N:5]1[C:13](=[O:14])[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[C:6]1=[O:15]

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 339432N-(3-Buten-1-yl)phthalimideHCID 516892Sodium Bicarbonate

생성물 1

HCID 3394332-[2-(oxiran-2-yl)ethyl]-2,3-dihydro-1H-isoindole-1,3-dione

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

70 g (350 mmol) 2-(but-3-enyl)-isoindolin-1,3-dione are dissolved in dichloromethane. The solution is cooled to ca. 0° C. and a suspension of 120.8 g (350 mmol) 50% 3-chloro-peroxy-benzoic acid in dichloromethane is added under cooling. The mixture is left standing without further cooling at room temperature for two days. After addition of 250 ml saturated NaHCO3 solution the organic phase is separated and washed three times each with 200 ml saturated NaHCO3 solution and once with water. The organic phase is dried over sodium sulfate and the solvent is removed under vacuum: yield 80 g.

후처리

  1. additionis added
  2. temperatureunder cooling
  3. waitThe mixture is left
  4. temperaturewithout further cooling at room temperature for two days
  5. customis separated
  6. washwashed three times each with 200 ml saturated NaHCO3 solution
  7. dry with materialThe organic phase is dried over sodium sulfate
  8. customthe solvent is removed under vacuum

출처 및 근거

ORD 기록
ord-b214c1b3a19d4f26a1c32cb490e950fe
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903118B1

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