N-methylhydroxylamine hydrochloride → 7-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

HRID 981113ノート

反応式

HRID 981113 の反応式
[CH2:1]([N:4]([CH2:8][C:9](=O)[CH3:10])[C:5](=[O:7])[CH3:6])[CH:2]=[CH2:3].C([O-])(=O)C.[Na+].Cl.[CH3:18][NH:19][OH:20]>O1CCOCC1.O>[C:5]([N:4]1[CH2:1][C:2]2([CH3:3])[CH:9]([CH2:10][O:20][N:19]2[CH3:18])[CH2:8]1)(=[O:7])[CH3:6]

参加物

6

反応物 3

HCID 77906N-methylhydroxylamine hydrochlorideHCID 517045Sodium AcetateHCID 15069994N-allyl-N-(2-oxopropyl)-acetamide

生成物 1

HCID 150700177-Acetyl-1,2-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

15.5 g (0.1 mol) of N-allyl-N-(2-oxopropyl)-acetamide are dissolved in 100 ml of dioxane, and 9 g of anhydrous sodium acetate and 9 g (0.108 mol) of N-methylhydroxylamine hydrochloride in 10 ml of water are added. The mixture is heated under reflux overnight and cooled and the salts are filtered off with suction and washed with dioxane. The filtrate is concentrated, the residue is taken up in 100 ml of water and K2CO3 is added. The mixture is extracted with CHCl3, the extract is dried over K2CO3 and concentrated and the residue is distilled.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux overnight
  3. temperaturecooled
  4. filtrationthe salts are filtered off with suction
  5. washwashed with dioxane
  6. concentrationThe filtrate is concentrated
  7. additionK2CO3 is added
  8. extractionThe mixture is extracted with CHCl3
  9. dry with materialthe extract is dried over K2CO3
  10. concentrationconcentrated
  11. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-1528066a30484e81b48142fc3ccc924b
出典データセット
uspto-grants-1991_02
特許番号
US04990517

反応ノート

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