Tert-Butylamine → HCID 19881210, compound

HRID 745307Notes

Reaction equation

HRID 745307 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([Cl:20])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.[C:21]([NH2:25])([CH3:24])([CH3:23])[CH3:22]>C(Cl)(Cl)Cl>[ClH:20].[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([NH:25][C:21]([CH3:24])([CH3:23])[CH3:22])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2

Participants

4

Reactant 2

HCID 6385Tert-ButylamineHCID 46787202-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

Product 1

HCID 19881210HCID 19881210, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A solution of 9,10-dimethoxy-2-chloro-6,7-dihydro-4H-pyrimido(6,1-a)isoquinolin-4-one (3.0 g) and tert.-butylamine (10.0 ml) in chloroform (75 ml) is heated under reflux for 16 hours. The solvent is evaporated under reduced pressure and the residue triturated with a dilute solution of sodium hydroxide to give a white precipitate. The precipitate is filtered, dried and converted into its hydrochloride by treating it in solution in ethanol with hydrochloric acid. The hydrochloride is crystallized from ethanol-ether mixture, yield 3.0 g, m.p. 265°-270° C.

Workup

  1. temperatureunder reflux for 16 hours
  2. customThe solvent is evaporated under reduced pressure
  3. customthe residue triturated with a dilute solution of sodium hydroxide
  4. customto give a white precipitate
  5. filtrationThe precipitate is filtered
  6. customdried
  7. additionby treating it in solution in ethanol with hydrochloric acid
  8. customThe hydrochloride is crystallized from ethanol-ether mixture, yield 3.0 g, m.p. 265°-270° C.

Sources & evidence

ORD record
ord-ecb861bbb26a4bcd9886879dfea14f1d
Source dataset
uspto-grants-1986_07
Patent number
US04598148

Reaction notes

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