N-methylhydroxylamine hydrochloride → Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

HRID 36697

反応式

HRID 36697 の反応式
[CH2:1]([N:5]([CH2:11][CH:12]=O)[C:6](=[O:10])[O:7][CH2:8][CH3:9])[CH:2]=[CH:3][CH3:4].C([O-])(=O)C.[Na+].Cl.[CH3:20][NH:21][OH:22]>O1CCOCC1.O>[CH3:20][N:21]1[O:22][CH:3]([CH3:4])[CH:2]2[CH:12]1[CH2:11][N:5]([C:6]([O:7][CH2:8][CH3:9])=[O:10])[CH2:1]2

参加物

6

反応物 3

HCID 77906N-methylhydroxylamine hydrochlorideHCID 517045Sodium AcetateHCID 53690408ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate

生成物 1

HCID 15070019Ethyl 2,4-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

18.4 g (0.1 mol) of ethyl N-(but-2-enyl)-N-(2-oxoethyl)-carbamate 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-c363c3f6a8394ce3b9913ed620fe0370
出典データセット
uspto-grants-1995_05
特許番号
US05416096

関連ノート

読み込み中…