Ethanolamine → HCID 53261092, compound

HRID 876137Notes

Reaction equation

HRID 876137 reaction equation
Cl[C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[CH:3]=1.[CH2:17]([CH2:19][NH2:20])[OH:18].CCN(C(C)C)C(C)C>Cl.CCCCO>[CH3:16][O:15][C:12]1[CH:13]=[CH:14][C:9]([NH:8][C:4]2[N:5]=[CH:6][N:7]=[C:2]([NH:20][CH2:19][CH2:17][OH:18])[CH:3]=2)=[CH:10][CH:11]=1

Participants

6

Reactant 3

HCID 700EthanolamineHCID 81531DiisopropylethylamineHCID 53410282HCID 53410282, compound

Product 1

HCID 53261092HCID 53261092, compound

Reagents, catalysts & solvents 2

HCID 2631-ButanolSolvent2×HCID 313Hydrochloric AcidSolvent

Conditions

Temperature
200 °C

Procedure

250 mg of 6-chloro-N-(4-methoxyphenyl)pyrimidine-4-amine in the form of a hydrochloride, 62 mg of ethanolamine and 296 mg of DIPEA were dissolved in 2 mL of n-BuOH and the mixture obtained was charged into a microwave vial and the vial obtained was heated to 200° C. for 45 minutes under microwave irradiation. Progress of the reaction was monitored by TLC. Upon termination of the reaction n-BuOH was evaporated. The evaporation residue was subjected to crystallization from an n-BuOH/EtOH solvent mixture.

Workup

  1. customthe mixture obtained
  2. additionwas charged into a microwave vial
  3. customthe vial obtained
  4. customwas evaporated
  5. customThe evaporation residue was subjected to crystallization from an n-BuOH/EtOH solvent mixture

Sources & evidence

ORD record
ord-25d1589a06794aa6a422f2956f5d7536
Source dataset
uspto-grants-2015_03
Patent number
US08986994B2

Reaction notes

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