Hydrochloric Acid → HCID 20338078, compound

HRID 1395767Notes

Reaction equation

HRID 1395767 reaction equation
[N:1]1[C:11]2[O:10][C:9]3[CH:12]=[CH:13][C:14]([CH:16]([CH3:20])[C:17]([OH:19])=[O:18])=[CH:15][C:8]=3[CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.Cl.C(=O)([O-])O.[Na+].[CH2:27](O)[CH3:28]>>[N:1]1[C:11]2[O:10][C:9]3[CH:12]=[CH:13][C:14]([CH:16]([CH3:20])[C:17]([O:19][CH2:27][CH3:28])=[O:18])=[CH:15][C:8]=3[CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][CH:2]=1

Participants

5

Reactant 4

HCID 313Hydrochloric AcidHCID 702Ethanol2×HCID 516892Sodium BicarbonateHCID 20338048HCID 20338048, compound

Product 1

HCID 20338078HCID 20338078, compound

Procedure

The mixture of 30 mg of 2-(5,6-dihydro benzo[b]pyrido[3,2-f]-oxepin-8-yl)-propionic acid in 0.5 ml of ethanol and 2 ml of ethanol saturated with hydrogen chloride gas was stirred at room temperature for 1 hour. The mixture was alkalified with saturated sodium hydrogencarbonate and extracted with chloroform. The extract was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain oily substance, which was chromatographed over silica gel, eluted with chloroform/benzene(1/4-1/3), and there was obtained 30 mg of ethyl 2-(5,6-dihydro benzo[b]pyrido-[3,2-f]oxepin-8-yl)-propionate as colorless oil.

Workup

  1. extractionextracted with chloroform
  2. washThe extract was washed with saturated sodium chloride solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off
  5. customto obtain oily substance, which
  6. customwas chromatographed over silica gel
  7. washeluted with chloroform/benzene(1/4-1/3)

Sources & evidence

ORD record
ord-228efde9e4964e359003bdbb7c3ac17d
Source dataset
uspto-grants-1980_05
Patent number
US04205170

Reaction notes

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