Pyridine → HCID 19775872、化合物

HRID 1613447

反応式

HRID 1613447 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[OH:6][CH2:7][CH2:8][NH:9][C:10](=[O:14])[O:11][CH2:12][CH3:13].N1C=CC=CC=1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH3:1][S:2]([O:6][CH2:7][CH2:8][NH:9][C:10](=[O:14])[O:11][CH2:12][CH3:13])(=[O:4])=[O:3]

参加物

6

反応物 3

HCID 1049PyridineHCID 31297Methanesulfonyl chlorideHCID 223805ethyl N-(2-hydroxyethyl)carbamate

生成物 1

HCID 19775872HCID 19775872、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

60 g of methanesulfonyl chloride are metered over approximately 30 minutes at 0° to +5° C. to a solution of 66.5 g of ethyl 2-hydroxyethylcarbamate, 43.5 g of pyridine and 1.9 g of 4-dimethylaminopyridine in 150 ml of methylene chloride, with stirring, and the mixture is stirred for 2 more hours at +5° C. and then for 16 hours at room temperature. The reaction mixture is filtered, the residue is washed with a small quantity of ethyl acetate, and the combined filtrates are washed with dilute hydrochloric acid and water. After the mixture has been dried over magnesium sulfate, the solvent mixture is removed completely by distillation in vacuo, which gives ethyl 2-methylsulfonyloxyethylcarbamate, nD20 1.4450.

後処理

  1. stirringthe mixture is stirred for 2 more hours at +5° C.
  2. filtrationThe reaction mixture is filtered
  3. washthe residue is washed with a small quantity of ethyl acetate
  4. washthe combined filtrates are washed with dilute hydrochloric acid and water
  5. dry with materialAfter the mixture has been dried over magnesium sulfate
  6. customthe solvent mixture is removed completely by distillation in vacuo, which

出典と根拠

ORDレコード
ord-d5c6d3b9d70e4c06980dc58cd703dd91
出典データセット
uspto-grants-1993_03
特許番号
US05192803

関連ノート

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