Hydrochloric Acid → HCID 20043143, compound

HRID 1762291Notes

Reaction equation

HRID 1762291 reaction equation
[CH3:1][NH:2][C:3]1[CH2:4][O:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8](=[O:10])[CH:9]=1.[ClH:15]>CO>[ClH:15].[CH3:1][NH:2][C:3]1[CH2:4][O:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8](=[O:10])[CH:9]=1

Participants

4

Reactant 2

HCID 313Hydrochloric Acid2×HCID 134460473-(Methylamino)-1-benzoxepin-5(2H)-one

Product 1

HCID 20043143HCID 20043143, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

19 g 3-methylamino-1-benzoxepin-5(2H)-one were suspended in 130 ml methanol, and gaseous hydrogen chloride was introduced into the suspension with stirring in order to convert it into its hydrochloride. The amine thereby goes into solution with warming. Subsequently approximately 40 ml methanol were distilled from the solution. The solution was allowed to stand to crystallize the hydrochloride which was formed, and the crystals which formed were removed by filtration. 22 g 3-methylamino-1-benzoxepin-5(2H)-one hydrochloride were obtained which were used without further purification in the following hydrogenation.

Workup

  1. temperaturewith warming
  2. distillationSubsequently approximately 40 ml methanol were distilled from the solution
  3. customto crystallize the hydrochloride which
  4. customwas formed
  5. customthe crystals which formed
  6. customwere removed by filtration

Sources & evidence

ORD record
ord-a205a25a394b419c90fc37aa46f536ef
Source dataset
uspto-grants-1989_05
Patent number
US04831167

Reaction notes

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