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

HRID 36685

反応式

HRID 36685 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-227c9b275f264cd383e3bb36421fbf18
出典データセット
uspto-grants-1995_05
特許番号
US05416096

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