Calcium Chloride → HCID 70443466, compound

HRID 1248446Notes

Reaction equation

HRID 1248446 reaction equation
[Br:1][C:2]1[C:13]2=[C:14]3[N:9]([CH:10]([CH3:15])[CH2:11][CH2:12]2)[CH:8]=[C:7]([C:16]([O-:18])=[O:17])[C:6](=[O:19])[C:5]3=[CH:4][C:3]=1[F:20].[Na+].[Cl-].[Ca+2:23].[Cl-]>O>[OH2:17].[Br:1][C:2]1[C:13]2=[C:14]3[N:9]([CH:10]([CH3:15])[CH2:11][CH2:12]2)[CH:8]=[C:7]([C:16]([O-:18])=[O:17])[C:6](=[O:19])[C:5]3=[CH:4][C:3]=1[F:20].[Ca+2:23].[Br:1][C:2]1[C:13]2=[C:14]3[N:9]([CH:10]([CH3:15])[CH2:11][CH2:12]2)[CH:8]=[C:7]([C:16]([O-:18])=[O:17])[C:6](=[O:19])[C:5]3=[CH:4][C:3]=1[F:20]

Participants

4

Reactant 2

HCID 5284359Calcium ChlorideHCID 23707684HCID 23707684, compound

Product 1

HCID 70443466HCID 70443466, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

Solutions of 1.7 g sodium 8-bromo-6,7-dihydro-9fluoro-5-methyl-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylate in 40 ml warm water and 2 g calcium chloride in 20 ml warm water were stirred together, heated on a steam bath for 15 minutes and cooled about 16 hours. The product was separated by filtration, washed with water and dried to provide light pink calcium 8-bromo-6,7-dihydro-9-fluoro-5-methyl-1-oxo-1H,5H-benzo[ij]quinolizine-2-carboxylate hydrate, m.p. >300° C. Analysis: Calculated for (C14H10BrFNO3)2Ca.1/2H2O: % C, 45.7; % H, 3.0; % N, 3.8; Found: % C, 45.7; % H, 3.2; % N, 3.8. The structural assignment was confirmed by infrared spectral analysis.

Workup

  1. temperatureheated on a steam bath for 15 minutes
  2. temperaturecooled about 16 hours
  3. customThe product was separated by filtration
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-989b2812c62047178021001d20c9bb38
Source dataset
uspto-grants-1985_06
Patent number
US04524148

Reaction notes

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