Hydrochloric Acid → HCID 178479086, compound

HRID 1602290Notes

Reaction equation

HRID 1602290 reaction equation
C([NH:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]2[C:24]3[C:19](=[N:20][CH:21]=[N:22][C:23]=3[NH:25][C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=3)[NH:18][N:17]=2)=[CH:11][CH:10]=1)(OC(C)(C)C)=O.Cl.C(OCC)C>CO>[ClH:32].[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]2[C:24]3[C:19](=[N:20][CH:21]=[N:22][C:23]=3[NH:25][C:26]3[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[CH:27]=3)[NH:18][N:17]=2)=[CH:11][CH:10]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 178452784HCID 178452784, compound

Product 1

HCID 178479086HCID 178479086, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 0.25 g (0.553 mmol) of 3-[4-(N-BOC-amino)-phenylamino]-4-(3-chloro-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine (see Example 65) and 10 ml of a 3N solution of hydrochloric acid in methanol is stirred at RT for 20 hours. Then 10 ml of diethyl ether are added, the reaction mixture is filtered and the filter residue is digested in hot methanol. After cooling, filtering and washing the filter residue with diethyl ether, the crystals are dried for 15 hours under a high vacuum at 100° C. and then left to stand under ambient conditions for 24 hours, yielding the title compound containing 10.97% hydrogen chloride and 4.34% water; m.p. 211-213° C.; EI-MS: (M)+ =351.

Workup

  1. filtrationthe reaction mixture is filtered
  2. temperatureAfter cooling
  3. filtrationfiltering
  4. washwashing the filter residue with diethyl ether
  5. customthe crystals are dried for 15 hours under a high vacuum at 100° C.
  6. waitleft
  7. waitto stand under ambient conditions for 24 hours

Sources & evidence

ORD record
ord-03a9b2e6e012415cbbbf5292b2ac48bc
Source dataset
uspto-grants-1999_11
Patent number
US05981533

Reaction notes

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