Ammonia → HCID 13672845, compound

HRID 652408Notes

Reaction equation

HRID 652408 reaction equation
Cl.[CH3:2][NH:3][CH:4]1[CH2:10][CH:9](O)[C:8]2[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=2[O:6][CH2:5]1.N>Cl>[CH3:2][NH:3][CH:4]1[CH:10]=[CH:9][C:8]2[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=2[O:6][CH2:5]1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 20197205HCID 20197205, compound

Product 1

HCID 13672845HCID 13672845, compoundYield 99.2%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

23.0 g of 3-methylamino-2,3,4,5-tetrahydro-1-benzoxepin-5-ol hydrochloride were heated to 100 degrees C. for 30 minutes with stirring in 50 ml of 32 percent aqueous hydrochloric acid solution. Subsequently, the solution was poured over 100 g of ice, and the mixture was rendered alkaline with 70 ml of 25 percent aqueous ammonia solution. The mixture was thereafter extracted once with 100 ml and four times with 25 ml portions of methylene chloride. The combined methylene chloride extracts were dried over sodium sulfate, and the solvent was distilled off under reduced pressure. 17.4 g of 3-methylamino-2,3-dihydro-1-benzoxepine were obtained as a colorless oil.

Workup

  1. extractionThe mixture was thereafter extracted once with 100 ml and four times with 25 ml portions of methylene chloride
  2. dry with materialThe combined methylene chloride extracts were dried over sodium sulfate
  3. distillationthe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-a1f5bb520c584909b7279a90d19434ed
Source dataset
uspto-grants-1987_06
Patent number
US04672062

Reaction notes

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