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

HRID 981100

反応式

HRID 981100 の反応式
C[O-].[Na+].Cl.[CH3:5][NH:6][OH:7].[Cl-].[Na+].[CH3:10][C:11](=[CH2:22])[CH2:12][N:13]([CH2:19][CH:20]=O)[C:14]([O:16][CH2:17][CH3:18])=[O:15]>CO.C1(C)C=CC=CC=1.O>[CH3:5][N:6]1[O:7][CH2:10][C:11]2([CH3:22])[CH:20]1[CH2:19][N:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:12]2

参加物

8

反応物 4

HCID 5234Sodium ChlorideHCID 77906N-methylhydroxylamine hydrochlorideHCID 10942334Sodium MethoxideHCID 15069992N-(2-Methylprop-2-enyl)-N-(2-oxoethyl)-urethane

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  1. filtrationis 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

出典と根拠

ORDレコード
ord-56d5b247e6aa4ff48e7fc105540a8a0a
出典データセット
uspto-grants-1991_02
特許番号
US04990517

関連ノート

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