Hydrochloric Acid → HCID 53946840, compound

HRID 262531Notes

Reaction equation

HRID 262531 reaction equation
Cl.Cl.[N+:3]([C:6]1[CH:7]=[CH:8][C:9]2[CH2:15][CH2:14][CH:13]([NH:16][CH3:17])[CH:12]=[CH:11][C:10]=2[CH:18]=1)([O-])=O.[OH-].[NH4+]>O>[NH2:3][C:6]1[CH:7]=[CH:8][C:9]2[CH2:15][CH2:14][CH:13]([NH:16][CH3:17])[CH:12]=[CH:11][C:10]=2[CH:18]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 86736535HCID 86736535, compound

Product 1

HCID 53946840HCID 53946840, compoundYield 104.1%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A mixture of 26 ml of fuming hydrochloric acid, 3.9 g of stannous chloride dihydrate and 1.3 g of 2-nitro-7-methylamino-6,7-dihydro [5H] benzocycloheptene hydrochloride was stirred at room temperature for 16 hours and was then cooled to 10° C. for the addition of 100 ml of water. The mixture was made alkaline at 10° C. with concentrated ammonium hydroxide and was then extracted 3 times with 50 ml of methylene chloride. The organic extracts were washed with water, dried over sodium sulfate and evaporated to dryness under reduced pressure to obtain 1 g of 2-amino-7-methylamino-6,7-dihydro [5H] benzocycloheptene in the form of a brown oil.

Workup

  1. customat 10° C.
  2. extractionwas then extracted 3 times with 50 ml of methylene chloride
  3. washThe organic extracts were washed with water
  4. dry with materialdried over sodium sulfate
  5. customevaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-25412f54023742408248b5486a32cd8d
Source dataset
uspto-grants-1979_05
Patent number
US04154852

Reaction notes

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