Sulfuric Acid → HCID 21420509, compound

HRID 441298Notes

Reaction equation

HRID 441298 reaction equation
C([NH:4][C:5]1(C(OCC)=O)[C:22](=[O:23])[N:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH:7]2[CH2:6]1)(=O)C.OS(O)(=O)=O.[OH-].[K+]>O>[NH2:4][CH:5]1[C:22](=[O:23])[N:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[CH:7]2[CH2:6]1

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 14797Potassium HydroxideHCID 53901600HCID 53901600, compound

Product 1

HCID 21420509HCID 21420509, compoundYield 97%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
130 °C

Procedure

To 34,5 g of 2-acetylamino-2-ethoxycarbonyl-3-oxo-1,2,3,13b-tetrahydro-9H-pyrrolo[1,2-a]-dibenzo[c,f] azepine (oil, Rf in toluene: ethanol (9:2) = 0.5) are added 170 ml water and 10 ml concentrated H2SO4. The mixture is refluxed at 130° C. for 18 hours, then cooled down and made alcaline with KOH. The mixture is extracted wtih methylenechloride and the extracts washed with water, dried and evaporated. Melting point 186°-188° C. Yield 97%.

Workup

  1. temperaturecooled down
  2. extractionThe mixture is extracted wtih methylenechloride
  3. washthe extracts washed with water
  4. customdried
  5. customevaporated

Sources & evidence

ORD record
ord-9184b2c9a3104bd985bb13d10ec30711
Source dataset
uspto-grants-1977_08
Patent number
US04039558

Reaction notes

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