Hydrochloric Acid → FK1052 hydrochloride

HRID 849464Notes

Reaction equation

HRID 849464 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.C(O)C.[ClH:26]>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:26]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 125368FK 1052

Product 1

HCID 9949384FK1052 hydrochlorideYield 93%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
10 °C

Procedure

(+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-on (100 g) was suspended in the mixture of ethanol (300 ml) and deionized water (300 ml), and 6 N hydrochloric acid (100 ml) was added thereto at an interior temperature of not less than 30° C. After the addition thereof, it was heated to an interior temperature of 65~75° C. and the precipitated crystals were dissolved. After the dissolution, it was clarified by filtration, and the filtration vessel and so forth were washed with 200 ml of deionized water. The filtrate and the washings was combined, cooled to a temperature of not higher than 10° C., and the precipitated crystals were collected by filtration, washed with water, and dried to obtain (+)8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one·hydrochloride as white crystals.

Workup

  1. additionwas added
  2. customat an interior temperature of not less than 30° C
  3. additionAfter the addition
  4. temperatureit was heated to an interior temperature of 65~75° C.
  5. dissolutionthe precipitated crystals were dissolved
  6. dissolutionAfter the dissolution, it
  7. filtrationwas clarified by filtration
  8. washthe filtration vessel and so forth were washed with 200 ml of deionized water
  9. filtrationthe precipitated crystals were collected by filtration
  10. washwashed with water
  11. customdried

Sources & evidence

ORD record
ord-7ab20d06543b4a5d9c12f90c6b8cd0ee
Source dataset
uspto-grants-2000_01
Patent number
US06013653

Reaction notes

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