Potassium Hydroxide → HCID 13308996, compound

HRID 2083376Notes

Reaction equation

HRID 2083376 reaction equation
[OH-].[K+].C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH:14]=[C:15]2[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[CH2:19][CH2:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]2=3)[CH2:9]1)=O)C>O.C(O)=C>[NH:8]1[CH2:13][CH2:12][O:11][CH:10]([CH:14]=[C:15]2[C:21]3[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=3[CH2:19][CH2:18][C:17]3[CH:26]=[CH:27][CH:28]=[CH:29][C:16]2=3)[CH2:9]1

Participants

5

Reactant 2

HCID 14797Potassium HydroxideHCID 20391648HCID 20391648, compound

Product 1

HCID 13308996HCID 13308996, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 11199Vinyl alcoholSolvent

Procedure

Potassium hydroxide (3.0 g) in water was added to the above-obtained 5-(4-ethoxycarbonylmorpholin-2-yl)methylidene-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2.49 g) in ethenol, and the resulting mixture was heated under reflux for 8 hours. After cooling, ethanol was distilled off and water was added to the resulting residue. The resultant mixture was extracted with chloroform. The chloroform extract was dried, evaporated and chromatographed to afford 5-(morpholin-2-yl)methylidene-10,11-dihydro-5H-dibenzo[a,d]cycloheptene as oily material. M.P., 221° - 224° C (oxalate).

Workup

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 8 hours
  3. temperatureAfter cooling
  4. distillationethanol was distilled off
  5. additionwater was added to the resulting residue
  6. extractionThe resultant mixture was extracted with chloroform
  7. extractionThe chloroform extract
  8. customwas dried
  9. customevaporated
  10. customchromatographed

Sources & evidence

ORD record
ord-3188a0c3c6424480ac148fceea3a0c00
Source dataset
uspto-grants-1978_04
Patent number
US04085210

Reaction notes

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