Hydrochloric Acid → HCID 10044403, compound

HRID 1905428Notes

Reaction equation

HRID 1905428 reaction equation
C([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[CH:19]=[C:18]3[C:13]([C:14](=[O:28])[C:15]([C:23]([O:25]CC)=[O:24])=[C:16]4[S:21][CH:20]([CH3:22])[N:17]43)=[CH:12][C:11]=2[Cl:29])[CH2:6][CH2:5]1)(=O)C.Cl.O.N>C(O)C>[Cl:29][C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:10]=1[N:7]1[CH2:8][CH2:9][NH:4][CH2:5][CH2:6]1)[N:17]1[CH:20]([CH3:22])[S:21][C:16]1=[C:15]([C:23]([OH:25])=[O:24])[C:14]2=[O:28]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 10478140HCID 10478140, compoundHCID 12896473Azane;hydrate

Product 1

HCID 10044403HCID 10044403, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Conditions

Temperature
50 °C

Procedure

A mixture of 610 mg of ethyl 7-(4-acetyl-1-piperazinyl)-6-chloro-1-methyl-4-oxo-4H-(1,3)thiazeto(3,2-a)quinoline-3-carboxylate, 12 ml of 5% hydrochloric acid and 3 ml of ethanol was heated with stirring on an oil bath of 100°-110° C. for 2 hours. After cooling to about 50° C., this was neutralized with 5% ammonia water. Crystals separated out were collected by filtration, washed with water, dried and recrystallized from N,N-dimethylformamide to give pale yellow crystals, m.p. not lower than 300° C. (decompn).

Workup

  1. temperaturewas heated
  2. customCrystals separated out
  3. filtrationwere collected by filtration
  4. washwashed with water
  5. customdried
  6. customrecrystallized from N,N-dimethylformamide
  7. customto give pale yellow crystals
  8. customm.p. not lower than 300° C.

Sources & evidence

ORD record
ord-48d6301a79fc4da0aa48c3ea41a12dfd
Source dataset
uspto-grants-1989_06
Patent number
US04843070

Reaction notes

Loading…