Sodium Hydroxide → Morphine

HRID 1487280Notes

Reaction equation

HRID 1487280 reaction equation
S(O)(O)(=O)=O.[CH:6]1[C:22]2[CH2:21][C@H:20]3[N:23]([CH2:25][CH2:26][C@@:12]45[C@H:19]3[CH:18]=[CH:17][C@H:15]([OH:16])[C@@H:13]4[O:14][C:10]([C:11]=25)=[C:8]([OH:9])[CH:7]=1)[CH3:24].[OH-].[Na+]>O>[CH:6]1[C:22]2[CH2:21][C@H:20]3[N:23]([CH2:25][CH2:26][C@@:12]45[C@H:19]3[CH:18]=[CH:17][C@H:15]([OH:16])[C@@H:13]4[O:14][C:10]([C:11]=25)=[C:8]([OH:9])[CH:7]=1)[CH3:24]

Participants

4

Reactant 2

HCID 14798Sodium Hydroxide3×HCID 546428064-31-3

Product 1

HCID 5288826Morphine

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
65 °C

Procedure

About 8.43 g of morphine sulfate and about 40 mL of water are added to an Easy Max™ set at 350 RPM agitation rate. The mixture becomes clear and is then heated to about 65° C. The pH is checked and determined to be about 5. About 10 mL of pre-made solution in water of 1 M NaOH is added to the mixture. Solids are formed. About 5 mL of pre-made solution in water of 1 M NaOH is added to the mixture. The pH is checked and determined to be about 6. A few NaOH pellets are added to the mixture. Heating and stirring is continued for about 2 hours. The mixture is then cooled to about 50° C., filtered under vacuum filtration and washed several times with water. The pH of the filtrate is checked and determined to be about 13. The filtrate is dried at about 45° C. under vacuum for about 12-24 hours. The resulting solids are analyzed by X-ray powder diffraction and determined to be morphine free base.

Workup

  1. customSolids are formed
  2. temperatureHeating
  3. temperatureThe mixture is then cooled to about 50° C.
  4. filtrationfiltered under vacuum filtration
  5. washwashed several times with water
  6. customThe filtrate is dried at about 45° C. under vacuum for about 12-24 hours

Sources & evidence

ORD record
ord-d3d50df5a6414fc38eff796ec55e1645
Source dataset
uspto-grants-2016_08
Patent number
US09428516B1

Reaction notes

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