Sodium Hydroxide → HCID 70128601, compound

HRID 369963Notes

Reaction equation

HRID 369963 reaction equation
[ClH:1].[CH2:2]([CH:4]1[CH2:10][NH:9][CH2:8][C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[O:5]1)[CH3:3].[N+:15]([O-])([O-:17])=[O:16].[K+].[OH-].[Na+]>S(=O)(=O)(O)O>[ClH:1].[N+:15]([C:12]1[CH:13]=[CH:14][C:6]2[O:5][CH:4]([CH2:2][CH3:3])[CH2:10][NH:9][CH2:8][C:7]=2[CH:11]=1)([O-:17])=[O:16]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 70126885HCID 70126885, compound

Product 1

HCID 70128601HCID 70128601, compound

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Procedure

2-Ethyl-2,3,4,5-tetrahydro-1,4-benzoxazapine hydrochloride (8.0 g, 37.3 mmol) was dissolved in concentrated sulfuric acid (100 ml) and to this was added potassium nitrate (3.77 g, 37.3 mmol) at 0° C. The mixture was allowed to stir for 5 min, dumped into ice, neutralized with 50% NaOH, and extracted with ethyl acetate (3×100 ml). The combined extracts were washed with water, dried over magnesium sulfate, filtered, and concentrated to an oil. The oil was dissolved in isopropanol and treated with isopropanol-HCl. The salt was filtered off and dried in vacuo (4.4 g, 46%), m.p. 238-240° C.

Workup

  1. extractionextracted with ethyl acetate (3×100 ml)
  2. washThe combined extracts were washed with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated to an oil
  6. dissolutionThe oil was dissolved in isopropanol
  7. additiontreated with isopropanol-HCl
  8. filtrationThe salt was filtered off
  9. customdried in vacuo (4.4 g, 46%), m.p. 238-240° C.

Sources & evidence

ORD record
ord-c9622212e90341faaadfb0d5a79ccb40
Source dataset
uspto-grants-2000_10
Patent number
US06140322

Reaction notes

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