Iodine → 4-(3-Iodo-4-methoxyphenyl)pyrrolidin-2-one

HRID 973699

반응식

HRID 973699 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:13][NH:12][C:11](=[O:14])[CH2:10]2)=[CH:5][CH:4]=1.[I:15](O)(=O)=O.II>C(O)(=O)C.O.S(=O)(=O)(O)O>[I:15][C:4]1[CH:5]=[C:6]([CH:9]2[CH2:13][NH:12][C:11](=[O:14])[CH2:10]2)[CH:7]=[CH:8][C:3]=1[O:2][CH3:1]

참가 물질

7

반응물 3

HCID 807IodineHCID 24345Iodic acidHCID 46562244-(4-Methoxyphenyl)pyrrolidin-2-one

생성물 1

HCID 145296994-(3-Iodo-4-methoxyphenyl)pyrrolidin-2-one수율 414.5%

시약·촉매·용매 3

HCID 176Acetic Acid용매HCID 962Water용매HCID 1118Sulfuric Acid용매

반응 조건

온도
80 °C

실험 절차

A solution of 19.1 g of 4-(4-methoxyphenyl)-pyrrolidin-2-one (100 mmol) in 200 ml of glacial acetic acid, 4.8 ml of water and 1.2 ml of concentrated sulfuric acid is combined with 3.44 g (19.55 mmol) of iodic acid and 8.64 g (70 mmol) of iodine and stirred at a bath temperature of 80° C. for 10 hours. Subsequently, the mixture is concentrated on a rotary evaporator up to onset of crystallization, cooled, the crystalline precipitate is suctioned off and recrystallized from ethyl acetate, thus obtaining 25.7 g (81% of theory) of 4-(3-iodo-4-methoxyphenyl)pyrrolidin-2-one, mp 158° C.

후처리

  1. concentrationSubsequently, the mixture is concentrated on a rotary evaporator up
  2. customto onset of crystallization
  3. temperaturecooled
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-26c59e9504d54bb5a2e995bb7b7c6dd0
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05064854

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