Water → Ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

HRID 345819

반응식

HRID 345819 반응식
Cl.[CH3:2][NH:3][OH:4].C[O-].[Na+].[CH2:8]([N:11]([CH:17]([CH3:20])[CH:18]=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:9]=[CH2:10].O>CO.C1(C)C=CC=CC=1>[CH3:2][N:3]1[O:4][CH2:10][CH:9]2[CH:18]1[CH:17]([CH3:20])[N:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:8]2

참가 물질

7

반응물 4

HCID 962WaterHCID 77906N-methylhydroxylamine hydrochlorideHCID 10942334Sodium MethoxideHCID 15069993Ethyl N-allyl-N-(1-oxoprop-2-yl)-carbamate

생성물 1

HCID 15070012Ethyl 2,8-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매2회

실험 절차

A methanolic methylhydroxylamine solution is prepared from 16.4 g (0.2 mol) of N-methylhydroxylamine hydrochloride in 33 ml of absolute methanol and 36 g (0.2 mol) of 30% strength sodium methylate solution, and the solution formed is diluted with 130 ml of toluene and added dropwise to 354 g (0.17 mol) of N-allyl-N-(1-oxoprop-2-yl)-urethane in 250 ml of toluene, which is heated under reflux using a water separator. The mixture is heated under reflux overnight, the product is extracted with dilute hydrochloric acid and the hydrochloric acid solution is rendered alkaline with K2CO3 and extracted with CHCl3. The extract is dried over K2CO3 and concentrated and the residue is distilled.

후처리

  1. customthe solution formed
  2. temperatureis heated
  3. temperatureunder reflux
  4. temperatureThe mixture is heated
  5. temperatureunder reflux overnight
  6. extractionthe product is extracted with dilute hydrochloric acid
  7. extractionextracted with CHCl3
  8. dry with materialThe extract is dried over K2CO3
  9. concentrationconcentrated
  10. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-7296856a4cf0446bbf47eb568577a18a
출처 데이터셋
uspto-grants-1991_10
특허 번호
US05059597

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