HCID 178425524, compound → HCID 178425525, compound

HRID 1602220Notes

Reaction equation

HRID 1602220 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:17]3[C:12](=[N:13][CH:14]=[N:15][C:16]=3[NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[CH:20]=3)[NH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1>C(O)C.Cl>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[C:17]3[C:12](=[N:13][CH:14]=[N:15][C:16]=3[NH:18][C:19]3[CH:24]=[CH:23][CH:22]=[C:21]([CH3:25])[CH:20]=3)[NH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1

Participants

4

Reactant 1

HCID 178425524HCID 178425524, compound

Product 1

HCID 178425525HCID 178425525, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolvent2×HCID 702EthanolSolvent2×

Conditions

Temperature
0 °C

Procedure

1.3 g of 3-(3-chloro-phenylamino)-4-(3-methyl-phenylamino)-1H-pyrazolo[3,4-d]-pyrimidine (see Example 5) are dissolved in 70 ml of ethanol and at room temperature 2 ml of a 4N solution of hydrogen chloride in ethanol are added thereto. After approximately 10 minutes' stirring, the HCl salt begins to crystallize out. The solution is cooled to 0° C. and the salt is crystallized out completely by the addition of ethyl ether, yielding colorless crystals of 3-(3-chloro-phenylamino)-4-(3-methyl-phenylamino)-1H-pyrazolo[3,4-d]pyrimidine hydrochloride; m.p. 260-263° C.

Workup

  1. additionare added
  2. customto crystallize out
  3. customthe salt is crystallized out completely by the addition of ethyl ether

Sources & evidence

ORD record
ord-be2bfcf7d2dc4922912c896b55d41082
Source dataset
uspto-grants-1999_11
Patent number
US05981533

Reaction notes

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