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

HRID 36693

반응식

HRID 36693 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e9c25c5ffd3943a2b66fece54b978100
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05416096

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