Pyridine → HCID 19775872, 화합물

HRID 1613447

반응식

HRID 1613447 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 19775872HCID 19775872, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d5c6d3b9d70e4c06980dc58cd703dd91
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05192803

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