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

HRID 1740379ノート

反応式

HRID 1740379 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9f888bf2e4a44ae0a1827dc41150fb45
出典データセット
uspto-grants-1999_10
特許番号
US05969138

反応ノート

読み込み中…