Hydroxylamine → HCID 178525219, compound

HRID 261728Notes

Reaction equation

HRID 261728 reaction equation
[C:1]12([CH2:12][C:11](=[O:13])[O:10][C:8](=[O:9])[CH2:7]1)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2.[NH2:14][OH:15].Cl.NO.C(=O)([O-])[O-].[Na+].[Na+]>>[OH:15][N:14]=[C:8]([OH:9])[CH2:7][C:1]1([CH2:12][C:11]([OH:10])=[O:13])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

5

Conditions

Temperature
70 °C

Procedure

50 g. 1,1-Cyclohexane-diacetic anhydride was introduced portionwise, while stirring, into an aqueous solution of hydroxylamine, prepared from 23.4 g. hydroxylamine hydrochloride and 21.12 g. sodium carbonate. After completion of the addition, the reaction mixture as heated for 2 hours at 70° C.; an oil separated out. After cooling, the pH was adjusted to 2 with 2N hydrochloric acid and the crystalline precipitate was filtered off with suction. The precipitate was washed with water, taken up in methanol, any undissolved material was removed and, after the addition of water, it was evaporated in a vacuum. There was obtained 45.5 g of 1,1-cyclohexane-diacetic acid N-hydroxyimide; m.p. 104° C.

Workup

  1. customprepared from 23.4 g
  2. additionAfter completion of the addition
  3. customan oil separated out
  4. temperatureAfter cooling
  5. filtrationthe crystalline precipitate was filtered off with suction
  6. washThe precipitate was washed with water
  7. customany undissolved material was removed
  8. additionafter the addition of water, it
  9. customwas evaporated in a vacuum

Sources & evidence

ORD record
ord-718d37905d8540cfb5ac8d0f7ba1eae3
Source dataset
uspto-grants-1979_05
Patent number
US04152326

Reaction notes

Loading…