Perchloric Acid → HCID 21998067, 화합물

HRID 1977444노트

반응식

HRID 1977444 반응식
[O:1]1[CH2:18][CH:2]1[CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15](=[O:16])[CH:14]=[CH:13][C:12]2=[O:17])=[CH:7][CH:6]=1.Cl(O)(=O)(=O)=[O:20].ClCCl.CO>CC(C)=O.O>[OH:20][CH:2]([CH2:18][OH:1])[CH2:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[C:12](=[O:17])[CH:13]=[CH:14][C:15]2=[O:16])=[CH:9][CH:10]=1

참가 물질

6

반응물 3

HCID 24247Perchloric AcidHCID 21226129Dichloromethane methanolHCID 219980621H-Pyrrole-2,5-dione, 1-[4-(oxiranylmethoxy)phenyl]-

생성물 1

HCID 21998067HCID 21998067, 화합물

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

To a suspension of N-(4-[2,3-epoxypropyl]oxyphenyl)maleimide (200 g, 0.816 mole) in 1360 ml of acetone was added perchloric acid (20 ml) in 660 ml of water. The reaction mixture was refluxed for 2 h, during which the solution became clear yellow (complete conversion on TLC, dichloromethane: methanol 90:10). After cooling, the acetone was removed under reduced pressure. Water was added to the resulting slurry which was stirred for 0.5 h. The solids were filtered off, washed with water and dissolved in THF (tetrahydrofuran). This solution was dried twice over anhydrous sodium sulfate, followed by concentration to dryness.

후처리

  1. temperatureThe reaction mixture was refluxed for 2 h, during which the solution
  2. temperatureAfter cooling
  3. customthe acetone was removed under reduced pressure
  4. additionWater was added to the resulting slurry which
  5. filtrationThe solids were filtered off
  6. washwashed with water
  7. dissolutiondissolved in THF (tetrahydrofuran)
  8. dry with materialThis solution was dried twice over anhydrous sodium sulfate
  9. concentrationfollowed by concentration to dryness

출처 및 근거

ORD 기록
ord-0423c2c9f6b54f89a41049d9c0568e20
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06232430B1

반응 노트

불러오는 중…