Hydrochloric Acid → 1,2-Dihydro-3-methyl-1-[4-(benzamido)butan-1-yl]-1,4,7b-triazacyclopent-[cd]inden-2-one.hydrochloride

HRID 619452Notes

Reaction equation

HRID 619452 reaction equation
[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:26])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[ClH:27]>CO>[CH3:1][C:2]1[N:3]=[C:4]2[CH:12]=[CH:11][CH:10]=[C:9]3[N:5]2[C:6]=1[C:7](=[O:26])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[ClH:27]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 211902531,2-Dihydro-3-methyl-1-[4-(benzamido)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one

Product 1

HCID 702128031,2-Dihydro-3-methyl-1-[4-(benzamido)butan-1-yl]-1,4,7b-triazacyclopent-[cd]inden-2-one.hydrochlorideYield 85.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 3.06 g (8.78 mmol) of 1,2-dihydro-3-methyl-1-[4-(benzamido)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one in 50 ml of methanol was added 0.88 ml of conc. HCl, then the solvent was distilled off. The residue was crystallized from methanol-acetone. The crystals were collected by filtration and washed with acetone to give 2.90 g of the object product (85.8%, colorless solid), m.p.173.0-175.5° C.

Workup

  1. distillationthe solvent was distilled off
  2. customThe residue was crystallized from methanol-acetone
  3. filtrationThe crystals were collected by filtration
  4. washwashed with acetone

Sources & evidence

ORD record
ord-83cbe8fa65364b9cbd431aa5c2bd5dc2
Source dataset
uspto-grants-1999_09
Patent number
US05958942

Reaction notes

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