Acetic Acid → HCID 178504606, compound

HRID 1891073Notes

Reaction equation

HRID 1891073 reaction equation
[Br:1][C:2]1[C:3]([OH:17])=[N:4][C:5]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([S:15][CH3:16])=[CH:11][CH:10]=2)=[N:6][CH:7]=1.C(O)(=[O:20])C>>[Br:1][C:2]1[C:3]([OH:17])=[N:4][C:5]([NH:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([CH3:16])=[O:20])=[CH:13][CH:14]=2)=[N:6][CH:7]=1

Participants

3

Reactant 2

HCID 176Acetic AcidHCID 178503248HCID 178503248, compound

Product 1

HCID 178504606HCID 178504606, compound

Procedure

11 g of 5-bromo-2-[4-(methylsulfanyl)phenylamino]pyrimidin-4-ol is suspended in 110 ml of glacial acetic acid. While being cooled with ice water, 4.6 ml of a 30% solution of hydrogen superoxide is added in drops. The mixture is stirred for 18 hours at room temperature and then suctioned off. The filter cake is washed twice with water and once with ethanol and dried at 60° C. in a vacuum. 8.75 g (75.7% of theory) of the product with a melting point of 240° C. (decomposition) is obtained.

Workup

  1. additionis added in drops
  2. washThe filter cake is washed twice with water and once with ethanol
  3. customdried at 60° C. in a vacuum
  4. custom8.75 g (75.7% of theory) of the product with a melting point of 240° C. (decomposition) is obtained

Sources & evidence

ORD record
ord-5f6cf336d19f4755b0d7d40339344443
Source dataset
uspto-grants-2013_08
Patent number
US08507510B2

Reaction notes

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