Hydrochloric Acid → HCID 86698046, compound

HRID 518895Notes

Reaction equation

HRID 518895 reaction equation
[C:1]([C:4]1[S:12][C:11]2[CH:10]=[N:9][C:8]([NH:13][C:14]3[N:18]([CH:19]([CH3:21])[CH3:20])[N:17]=[C:16]([CH:22]4[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]4)[CH:15]=3)=[N:7][C:6]=2[C:5]=1[C:35]1[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=1[O:41][C:42]([F:45])([F:44])[F:43])(=[O:3])[NH2:2].[ClH:46]>C(OCC)(=O)C>[ClH:46].[NH:25]1[CH2:24][CH2:23][CH:22]([C:16]2[CH:15]=[C:14]([NH:13][C:8]3[N:9]=[CH:10][C:11]4[S:12][C:4]([C:1]([NH2:2])=[O:3])=[C:5]([C:35]5[CH:40]=[CH:39][CH:38]=[CH:37][C:36]=5[O:41][C:42]([F:43])([F:44])[F:45])[C:6]=4[N:7]=3)[N:18]([CH:19]([CH3:21])[CH3:20])[N:17]=2)[CH2:27][CH2:26]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 86698048HCID 86698048, compound

Product 1

HCID 86698046HCID 86698046, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

220 mg of 2-methylpropan-2-yl 4-[5-({6-carbamoyl-7-[2-(trifluoromethoxy)phenyl]thieno[3,2-d]pyrimidin-2-yl}amino)-1-(propan-2-yl)-1H-pyrazol-3-yl]piperidine-1-carboxylate are added to 5 ml of a 1N solution of hydrochloric acid in ethyl acetate at a temperature of about 20° C. and the mixture is left to stir for 30 minutes. A further addition of 3 ml of the 1N acid solution is carried out and the mixture is left to stir for 15 h. After concentration of the mixture under reduced pressure, a solid is obtained which is washed successively with dichloromethane and then with ether. The solid is dried under reduced pressure, so as to obtain 139 mg of 2-{[3-(piperidin-4-yl)-1-(propan-2-yl)-1H-pyrazol-5-yl]amino}-7-[2-(trifluoromethoxy)phenyl]thieno[3,2-d]pyrimidine-6-carboxamide hydrochloride.

Workup

  1. waitthe mixture is left
  2. waitthe mixture is left
  3. stirringto stir for 15 h
  4. customAfter concentration of the mixture under reduced pressure, a solid is obtained which
  5. washis washed successively with dichloromethane
  6. customThe solid is dried under reduced pressure

Sources & evidence

ORD record
ord-20502d31c195483998baaee6e1e958e8
Source dataset
uspto-grants-2015_08
Patent number
US09115140B2

Reaction notes

Loading…