Diethyl Ether → 1-(4-Chlorophenyl)-3-mesyloxymethyl-2-pyrrolidinone

HRID 1740379노트

반응식

HRID 1740379 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:17][CH2:16][CH:15]([CH2:18][OH:19])[C:14]2=[O:20])=[CH:9][CH:8]=1.C(N(CC)CC)C.C(OCC)C>ClCCl>[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([N:13]2[CH2:17][CH2:16][CH:15]([CH2:18][O:19][S:2]([CH3:1])(=[O:4])=[O:3])[C:14]2=[O:20])=[CH:9][CH:8]=1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 218386441-(4-Chlorophenyl)-3-(hydroxymethyl)pyrrolidin-2-one

생성물 1

HCID 218386401-(4-Chlorophenyl)-3-mesyloxymethyl-2-pyrrolidinone수율 95.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Under ice-cooling, 14.0 g of methanesulfonyl chloride was added dropwise to a solution of 23.2 g of 1-(4-chlorophenyl)-3-hydroxymethyl-2-pyrrolidinone and 12.5 g of triethylamine in 200 mL of dichloromethane. After 2 hours, the reaction mixture was washed with water, dried over anhydrous magnesium sulfate and concentrated to give crystals. The crystals were sludged with diethyl ether and collected by filtration. The crystals were washed with diethyl ether and dried in vacuo to give 29.8 g of the title compound.

후처리

  1. temperatureUnder ice-cooling
  2. washthe reaction mixture was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customto give crystals
  6. filtrationcollected by filtration
  7. washThe crystals were washed with diethyl ether
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-9f888bf2e4a44ae0a1827dc41150fb45
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05969138

반응 노트

불러오는 중…