Hydrochloric Acid → FK1052 hydrochloride

HRID 849461Notes

Reaction equation

HRID 849461 reaction equation
[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]2[C:11](=[O:22])[CH:12]([CH2:15][C:16]3[N:17]=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:13][CH2:14][C:3]=12.[ClH:23]>C(O)C.O>[CH3:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]2[C:11](=[O:22])[CH:12]([CH2:15][C:16]3[N:17]=[CH:18][NH:19][C:20]=3[CH3:21])[CH2:13][CH2:14][C:3]=12.[ClH:23]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 125368FK 1052

Product 1

HCID 9949384FK1052 hydrochlorideYield 82%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

(+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (8.0 g) was dissolved in ethanol (80 ml) and water (72 ml), and 6 N hydrochloric acid (8 ml) was added thereto at an interior temperature of 20~30° C., and it was agitated at the same temperature for 1 hr. It was clarified by filtration, and the container and so forth was washed with ethanol (8 ml). Water (272 ml) was dripped therein at a temperature of 20~30° C. over the course of 20 min, and the seed crystals (0.016 g) were added thereto, and it was agitated at the same temperature for 3 hr, cooled to 0~5° C., and agitated for 3 hr. The precipitated crystals were collected by filtration, washed with water (32 ml), and thereafter dried overnight under vacuum to obtain (+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one·hydrochloride.

Workup

  1. filtrationIt was clarified by filtration
  2. washthe container and so forth was washed with ethanol (8 ml)
  3. additionat a temperature of 20~30° C. over the course of 20 min, and the seed crystals (0.016 g) were added
  4. stirringit was agitated at the same temperature for 3 hr
  5. temperaturecooled to 0~5° C.
  6. stirringagitated for 3 hr
  7. filtrationThe precipitated crystals were collected by filtration
  8. washwashed with water (32 ml)
  9. customdried overnight under vacuum

Sources & evidence

ORD record
ord-0199ee6c34714cd0924102221ffb2177
Source dataset
uspto-grants-2000_01
Patent number
US06013653

Reaction notes

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