Methanol → HCID 20436395, compound

HRID 647488Notes

Reaction equation

HRID 647488 reaction equation
[ClH:1].[NH2:2][C:3]1[C:4](Br)=[N:5][C:6]2[CH2:12][CH2:11][N:10]([CH2:13][CH3:14])[CH2:9][CH2:8][C:7]=2[N:15]=1.[Na].[CH3:18]O>>[ClH:1].[ClH:1].[NH2:2][C:3]1[C:4]([CH3:18])=[N:5][C:6]2[CH2:12][CH2:11][N:10]([CH2:13][CH3:14])[CH2:9][CH2:8][C:7]=2[N:15]=1

Participants

4

Reactant 3

HCID 887MethanolHCID 5360545SodiumHCID 20436384HCID 20436384, compound

Product 1

HCID 20436395HCID 20436395, compound

Conditions

Temperature
150 °C

Procedure

1 gm (3.3 mmols) of 2-amino-3-bromo-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine hydrochloride were admixed with a solution of 1 gm (43.5 mmols) of sodium in 50 ml of methanol, and the mixture was stirred for 10 hours at 150° C. in an autoclave. Thereafter, the reaction mixture was evaporated, the residue was taken up in 2 N sodium hydroxide, and the solution was extracted with chloroform. The chloroform extract solution was evaporated, the residue was dissolved in acetone, and the solution was admixed with ethanolic hydrochloric acid, yielding the hydrochloride in the form of white crystals.

Workup

  1. customThereafter, the reaction mixture was evaporated
  2. extractionthe solution was extracted with chloroform
  3. extractionThe chloroform extract solution
  4. customwas evaporated
  5. dissolutionthe residue was dissolved in acetone

Sources & evidence

ORD record
ord-ad2bbcaa835c4fb0b465634054001985
Source dataset
uspto-grants-1983_10
Patent number
US04409220

Reaction notes

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