Calcium Carbonate → HCID 67821607, compound

HRID 1742806Notes

Reaction equation

HRID 1742806 reaction equation
[OH:1][CH:2]([CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=1)[CH2:3][N:4]1[CH2:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[F:20][C:21]1[CH:26]=[CH:25][C:24]([CH:27]([C:32]2[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=2)[CH2:28][CH2:29][CH2:30]Cl)=[CH:23][CH:22]=1.C(=O)([O-])[O-].[Ca+2]>C1(C)C=CC=CC=1>[F:20][C:21]1[CH:22]=[CH:23][C:24]([CH:27]([C:32]2[CH:33]=[CH:34][C:35]([F:38])=[CH:36][CH:37]=2)[CH2:28][CH2:29][CH2:30][N:7]2[CH2:8][CH2:9][CH2:10][N:4]([CH2:3][CH:2]([OH:1])[CH2:11][O:12][C:13]3[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=3)[CH2:5][CH2:6]2)=[CH:25][CH:26]=1

Participants

5

Reactant 3

HCID 10112Calcium CarbonateHCID 768201,1'-(4-Chlorobutylidene)bis(4-fluorobenzene)HCID 19005868HCID 19005868, compound

Product 1

HCID 67821607HCID 67821607, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

5.9 g (0.022 mol) of 1-[2-hydroxy-3-(4-fluorophenoxy)propyl]homopiperazine and 6.2 g (0.022 mol) of 4,4-bis(4-fluorophenyl)butyl chloride were dissolved with 3.2 g of calcium carbonate in 100 ml of toluene and heated to boiling under reflux with stirring for 2.5 h. After cooling, filtration with suction was carried out, the solvent was removed by distillation under reduced pressure, and the residue was purified by column chromatography. (Silica gel, eluent methylene chloride with 4% methanol). Yield 4.0 g, oxalate, C30H35F3N2O2.2 C2H2O4, melting point 160°-165° C.

Workup

  1. temperatureheated
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. filtrationfiltration with suction
  5. customthe solvent was removed by distillation under reduced pressure
  6. customthe residue was purified by column chromatography

Sources & evidence

ORD record
ord-9f408cdf5eaf40728796f151162c943f
Source dataset
uspto-grants-1994_08
Patent number
US05342839

Reaction notes

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