Hydrochloric Acid → HCID 18352683, compound

HRID 429726Notes

Reaction equation

HRID 429726 reaction equation
C([N:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][C:12]([C:14]2[CH:15]=[CH:16][C:17]3[O:23][CH2:22][CH2:21][N:20](C(=O)C)[CH2:19][C:18]=3[CH:27]=2)=[O:13])[CH2:6][CH2:5]1)(=O)C.[ClH:28]>>[ClH:28].[ClH:28].[NH:4]1[CH2:9][CH2:8][CH:7]([CH2:10][CH2:11][C:12]([C:14]2[CH:15]=[CH:16][C:17]3[O:23][CH2:22][CH2:21][NH:20][CH2:19][C:18]=3[CH:27]=2)=[O:13])[CH2:6][CH2:5]1

Participants

3

Reactant 2

HCID 313Hydrochloric AcidHCID 15552339HCID 15552339, compound

Product 1

HCID 18352683HCID 18352683, compound

Procedure

3-(1-Acetylpiperidin-4-yl)-1-(4-acetyl-2,3,4,5-tetrahydro-1,4-benzoxazepin-7-yl)-1-propanone (1.5 g) obtained in Example 1 was dissolved in 30 ml of conc. hydrochloric acid, and the mixture was stirred for 16 hours under reflux. Excess volume of the conc. hydrochloric acid was distilled off under reduced pressure and ethanol was added to the residue. The resultant crystals were collected by filtration, and washed with ethanol. The crystals were dried under reduced pressure to give 1.4 g of the title compound as colorless scaly crystals, m.p. >300° C.

Workup

  1. temperatureunder reflux
  2. distillationExcess volume of the conc. hydrochloric acid was distilled off under reduced pressure and ethanol
  3. additionwas added to the residue
  4. filtrationThe resultant crystals were collected by filtration
  5. washwashed with ethanol
  6. customThe crystals were dried under reduced pressure

Sources & evidence

ORD record
ord-67e71e64fb3542619609ab5e1d5d5743
Source dataset
uspto-grants-2001_11
Patent number
US06319916B1

Reaction notes

Loading…