Hydrochloric Acid → HCID 86698045, compound

HRID 518894Notes

Reaction equation

HRID 518894 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][CH3:42])(=[O:3])[NH2:2].[ClH:43]>O1CCOCC1>[ClH:43].[CH3:42][O:41][C:36]1[CH:37]=[CH:38][CH:39]=[CH:40][C:35]=1[C:5]1[C:6]2[N:7]=[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][NH:25][CH2:24][CH2:23]4)[CH:15]=3)[N:9]=[CH:10][C:11]=2[S:12][C:4]=1[C:1]([NH2:2])=[O:3]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 71745766HCID 71745766, compound

Product 1

HCID 86698045HCID 86698045, compound

Reagents, catalysts & solvents 1

HCID 312751,4-DioxaneSolvent

Procedure

Note 3: Example I-61 was prepared from Example I-52 according to the following method: 140 mg of 2-methylpropan-2-yl 4-[5-{[6-carbamoyl-7-(2-methoxyphenyl)thieno[3,2-d]pyrimidin-2-yl]amino}-1-(propan-2-yl)-1H-pyrazol-3-yl]piperidine-1-carboxylate are added to a solution of 4 ml of 4N hydrochloric acid in dioxane at a temperature of about 20° C. and the mixture is left to stir for 30 minutes. After concentration of the mixture under reduced pressure, a solid is obtained which is washed successively with ethyl ether, with dichloromethane, with dioxane and to finish with dichloromethane. The solid is dried under reduced pressure, so as to obtain 112 mg of 7-(2-methoxyphenyl)-2-{[3-(piperidin-4-yl)-1-(propan-2-yl)-1H-pyrazol-5-yl]amino}thieno[3,2-d]pyrimidine-6-carboxamide hydrochloride.

Workup

  1. waitthe mixture is left
  2. customAfter concentration of the mixture under reduced pressure, a solid is obtained which
  3. washis washed successively with ethyl ether, with dichloromethane, with dioxane
  4. customThe solid is dried under reduced pressure

Sources & evidence

ORD record
ord-b2bf261bfdd04b87ab45c9bc1d2545a3
Source dataset
uspto-grants-2015_08
Patent number
US09115140B2

Reaction notes

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