Water → Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

HRID 36681

반응식

HRID 36681 반응식
C[O-].[Na+].Cl.[CH3:5][NH:6][OH:7].[CH3:8][C:9](=[CH2:20])[CH2:10][N:11]([CH2:17][CH:18]=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13].O>CO.C1(C)C=CC=CC=1>[CH3:5][N:6]1[O:7][CH2:8][C:9]2([CH3:20])[CH:18]1[CH2:17][N:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH2:10]2

참가 물질

7

반응물 4

HCID 962WaterHCID 77906N-methylhydroxylamine hydrochlorideHCID 10942334Sodium MethoxideHCID 15069992N-(2-Methylprop-2-enyl)-N-(2-oxoethyl)-urethane

생성물 1

HCID 15070010Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

시약·촉매·용매 2

HCID 887Methanol용매HCID 1140Toluene용매

실험 절차

21.7 g of 30% strength sodium methylate solution are added dropwise to 10 g (0.12 mol) of N-methylhydroxylamine hydrochloride in 26 ml of methanol. The sodium chloride is filtered off with suction and washed with 8 ml of methanol and 80 ml of toluene. This solution is added dropwise to 19.2 g (0.11 mol) of N-(2-methyl-prop-2-enyl)-N-(2-oxoethyl)-urethane, which is heated under reflux in 160 ml of toluene using a water separator. The mixture is heated under reflux overnight, the product is extracted with 160 ml of 10% strength hydrochloric acid and the hydrochloric acid solution is rendered alkaline with potassium carbonate and extracted with six portions, of 200 ml of CHCl3. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

후처리

  1. filtrationThe sodium chloride is filtered off with suction
  2. washwashed with 8 ml of methanol and 80 ml of toluene
  3. temperatureis heated
  4. temperatureThe mixture is heated
  5. temperatureunder reflux overnight
  6. extractionthe product is extracted with 160 ml of 10% strength hydrochloric acid
  7. extractionextracted with six portions, of 200 ml of CHCl3
  8. dry with materialThe extracts are dried over K2CO3
  9. concentrationconcentrated
  10. distillationthe residue is distilled

출처 및 근거

ORD 기록
ord-7020e83ef5a14745ace0469bb96f35b9
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416096

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