Hydrochloric Acid → HCID 15840429, compound

HRID 2289312Notes

Reaction equation

HRID 2289312 reaction equation
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH2:21][C:22]([N:24]3[CH2:29][CH2:28][CH:27]([N:30]4[C:35]5[CH:36]=[CH:37][CH:38]=[CH:39][C:34]=5[CH2:33][O:32][C:31]4=[O:40])[CH2:26][CH2:25]3)=[O:23])=[C:17]([C:41]([F:44])([F:43])[F:42])[CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl>CCOC(C)=O>[NH:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([CH2:21][C:22]([N:24]3[CH2:25][CH2:26][CH:27]([N:30]4[C:35]5[CH:36]=[CH:37][CH:38]=[CH:39][C:34]=5[CH2:33][O:32][C:31]4=[O:40])[CH2:28][CH2:29]3)=[O:23])=[C:17]([C:41]([F:44])([F:42])[F:43])[CH:16]=2)[CH2:10][CH2:9]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 18700126HCID 18700126, compound

Product 1

HCID 15840429HCID 15840429, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
0 °C

Procedure

Into a stirred solution of 1-(1-(4-(1-tert-butyloxycarbonyl-4-piperidinyloxy)-2-(trifluoromethyl)phenylacetyl)piperidin-4-yl)-4H-3,1-benzoxazin-2(1H)-one (0.35 g, 0.51 mmol) from Step 7 above in EtOAc (25 mL) at 0° C. was bubbled HCl gas for 15 min. The resulting suspension was stirred at 0° C. for 45 min. Excess HCl was removed by bubbling argon though the mixture for 15 min. The solvent was removed under reduced pressure and the residue was dissolved in CH2Cl2. The solvent was evaporated under reduced pressure to give the hydrochloride salt of the title compound as an amorphous solid.

Workup

  1. customExcess HCl was removed
  2. customby bubbling argon though the mixture for 15 min
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in CH2Cl2
  5. customThe solvent was evaporated under reduced pressure

Sources & evidence

ORD record
ord-a43bde71a37a45148651b4de2e190df9
Source dataset
uspto-grants-2000_07
Patent number
US06090805

Reaction notes

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