Methanesulfonyl chloride → 2-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl methanesulfonate

HRID 1859940노트

반응식

HRID 1859940 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][N:9]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:11]2[C:10]1=[O:19]>ClCCl.C(N(CC)CC)C>[CH3:1][S:2]([O:6][CH2:7][CH2:8][N:9]1[C:13](=[O:14])[C:12]2=[CH:15][CH:16]=[CH:17][CH:18]=[C:11]2[C:10]1=[O:19])(=[O:4])=[O:3]

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 77499N-(2-Hydroxyethyl)phthalimide

생성물 1

HCID 186258622-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)ethyl methanesulfonate수율 67.7%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

After methanesulfonyl chloride (12.7 g) was added to a solution of N-(2-hydroxyethyl)phthalimide (19.1 g) in anhydrous dichloromethane (200 ml), triethylamine (20 ml) was added dropwise to the mixture in an ice bath. The mixture was stirred at ambient temperature for 4 hours. At the end of this time the reaction mixture was concentrated under reduced pressure. The residual solid was washed with ethyl acetate and water and then recrystallized from ethyl acetate to afford the desired compound (18.2 g).

후처리

  1. additionwas added dropwise to the mixture in an ice bath
  2. concentrationAt the end of this time the reaction mixture was concentrated under reduced pressure
  3. washThe residual solid was washed with ethyl acetate and water
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-68ef658b092743ee90ebd74af6f51dcd
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06528525B1

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