Hydrochloric Acid → HCID 14988016, compound

HRID 892734Notes

Reaction equation

HRID 892734 reaction equation
Cl.[CH3:2][C:3]1([CH3:9])[NH:8][CH2:7][CH2:6][S:5][CH2:4]1.[N:10]([O-])=[O:11].[Na+].C(=O)([O-])[O-].[K+].[K+]>O>[N:10]([N:8]1[CH2:7][CH2:6][S:5][CH2:4][C:3]1([CH3:9])[CH3:2])=[O:11]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 149880153,3-DimethylthiomorpholineHCID 23668193Sodium Nitrite

Product 1

HCID 14988016HCID 14988016, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

12 ml of 10N HCl are added with cooling to a mixture of 15.7 g of 3,3-dimethyltetrahydro-1,4-thiazine (step c) and 60 ml of ice-water. A solution of 12.4 g of sodium nitrite in 40 ml of water is then added dropwise at 4° to 6° C. The mixture is subsequently stirred at room temperature for 4 hours, rendered alkaline with potassium carbonate and extracted by shaking with ethyl acetate. The organic phase is dried and concentrated in a water jet vacuum. Yield: 17.5 g; M.p.: yellow oil.

Workup

  1. extractionextracted
  2. stirringby shaking with ethyl acetate
  3. customThe organic phase is dried
  4. concentrationconcentrated in a water jet vacuum

Sources & evidence

ORD record
ord-95a491b694c84b4da0c244312a2a1310
Source dataset
uspto-grants-1992_06
Patent number
US05120732

Reaction notes

Loading…