Sodium Hydroxide → HCID 18378526, compound

HRID 2298815Notes

Reaction equation

HRID 2298815 reaction equation
C([N:4]1[CH2:10][CH2:9][CH2:8][N:7]([CH3:11])[C:6]2[N:12]=[CH:13][CH:14]=[CH:15][C:5]1=2)(=O)C.[OH-].[Na+]>Cl>[CH3:11][N:7]1[CH2:8][CH2:9][CH2:10][NH:4][C:5]2[CH:15]=[CH:14][CH:13]=[N:12][C:6]1=2

Participants

4

Reactant 2

HCID 14798Sodium HydroxideHCID 157315631-(5-Methyl-2,3,4,5-tetrahydro-1H-pyrido[2,3-b][1,4]diazepin-1-yl)ethan-1-one

Product 1

HCID 18378526HCID 18378526, compoundYield 96.2%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

A solution of 1-acetyl-5-methyl-2,3,4,5-tetrahydro-1H-pyrido[2,3-b][1,4]diazepine (1.7 g) in 6N hydrochloric acid (60 ml) was heated at 100° C. for 6 hours. After cooling, the mixture was basified with aqueous sodium hydroxide and extracted with ethyl acetate. The extracted organic layer was washed with brine and dried over sodium sulfate and concentrated in vacuo. The residue was washed with hexane to give 5-methyl-2,3,4,5-tetrahydro-1H-pyrido[2,3-b][1,4]diazepine (1.3 g).

Workup

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe extracted organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. washThe residue was washed with hexane

Sources & evidence

ORD record
ord-f4bd085952d848ae8b9f5ff0e20dc6a8
Source dataset
uspto-grants-2002_12
Patent number
US06495542B1

Reaction notes

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