Acetic Anhydride → HCID 23335270, compound

HRID 903845Notes

Reaction equation

HRID 903845 reaction equation
[CH2:1]([C:4]1[C:9]([CH:10]=[N:11]O)=[CH:8][C:7]2[O:13][CH2:14][O:15][C:6]=2[CH:5]=1)[CH2:2][CH3:3].C(OC(=O)C)(=O)C>O>[CH2:1]([C:4]1[C:9]([C:10]#[N:11])=[CH:8][C:7]2[O:13][CH2:14][O:15][C:6]=2[CH:5]=1)[CH2:2][CH3:3]

Participants

4

Procedure

62.2 g (0.3 mol) of 6-n-propyl-3,4-methylenedioxybenzaldoxime were stirred with 400 ml of acetic anhydride for 3 hours under reflux, and the reaction solution was cooled and poured into water. It was left to stand for 2 hours and then extracted with toluene, and the organic phase was washed first with water, then with sodium bicarbonate solution and again with water until neutral. After drying over sodium sulphate, the organic phase was concentrated and distilled. 38 g (67% of theory) of boiling point 116° C./3 mm Hg were obtained.

Workup

  1. temperatureunder reflux
  2. temperaturethe reaction solution was cooled
  3. waitIt was left
  4. extractionextracted with toluene
  5. washthe organic phase was washed first with water
  6. dry with materialAfter drying over sodium sulphate
  7. concentrationthe organic phase was concentrated
  8. distillationdistilled
  9. custom38 g (67% of theory) of boiling point 116° C./3 mm Hg were obtained

Sources & evidence

ORD record
ord-f9a2647a325b42c4bf273e0f5438d77f
Source dataset
uspto-grants-1980_10
Patent number
US04229445

Reaction notes

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