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

HRID 1859940ノート

反応式

HRID 1859940 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-68ef658b092743ee90ebd74af6f51dcd
出典データセット
uspto-grants-2003_03
特許番号
US06528525B1

反応ノート

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