Ethanol → HCID 12837721, compound

HRID 1447402Notes

Reaction equation

HRID 1447402 reaction equation
C([N:6]1[CH2:23][CH2:22][N:9]2[C:10]3[CH:21]=[CH:20][CH:19]=[CH:18][C:11]=3[CH2:12][N:13]3[CH:17]=[CH:16][CH:15]=[C:14]3[CH:8]2[CH2:7]1)(OCC)=[O:2].[CH2:24]([OH:26])[CH3:25].[OH-].[K+].[C:29]([O:32]CC)(=[O:31])[CH3:30]>>[C:29]([OH:32])(=[O:31])/[CH:30]=[CH:25]\[C:24]([OH:2])=[O:26].[CH2:7]1[CH:8]2[C:14]3[N:13]([CH:17]=[CH:16][CH:15]=3)[CH2:12][C:11]3[CH:18]=[CH:19][CH:20]=[CH:21][C:10]=3[N:9]2[CH2:22][CH2:23][NH:6]1

Participants

5

Reactant 4

HCID 702EthanolHCID 8857Ethyl AcetateHCID 14797Potassium HydroxideHCID 13163313HCID 13163313, compound

Product 1

HCID 12837721HCID 12837721, compound

Procedure

The mixture of 930 mg of 2-carbethoxy-1,3,4,14b-tetrahydro-10H--pyrazino[1,2-a]pyrrolo[2,1-c][1,4]-benzodiazepine, 40 ml of ethanol and 20 ml of 20% aqueous potassium hydroxide is refluxed for 2 days. After cooling, it is diluted with ethyl acetate, washed with water, dried and evaporated. The residue is taken up in diethyl ether and the solution combined with 0.55 g of maleic acid in the minimum amount of acetone. The precipitate formed is collected and washed with diethyl ether, to yield the 1,3,4,14b-tetrahydro-2H,10H-pyrazino[1,2-a]pyrrolo[2,1-c][1,4]-benzodiazepine maleate melting at 173°-175°.

Workup

  1. temperatureis refluxed for 2 days
  2. temperatureAfter cooling
  3. washwashed with water
  4. customdried
  5. customevaporated
  6. customThe precipitate formed
  7. customis collected
  8. washwashed with diethyl ether

Sources & evidence

ORD record
ord-b90b455fd9a54b5fbfbcbe1aaf03e5b8
Source dataset
uspto-grants-1982_02
Patent number
US04316900

Reaction notes

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