Hydrochloric Acid → 1,2-Dihydro-3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl]-1,4,7b-triazacyclopent(cd]inden-2-one.hydrochloride

HRID 619449Notes

Reaction equation

HRID 619449 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:28])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][NH:19][S:20]([CH2:23][C:24]([F:27])([F:26])[F:25])(=[O:22])=[O:21].[ClH:29]>CO>[ClH:29].[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:28])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][NH:19][S:20]([CH2:23][C:24]([F:26])([F:25])[F:27])(=[O:22])=[O:21]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 702131501,2-Dihydro-3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl)-1,4,7b-triazacyclopent[cd]inden-2-one

Product 1

HCID 702131491,2-Dihydro-3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl]-1,4,7b-triazacyclopent(cd]inden-2-one.hydrochlorideYield 94.1%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of 702 mg (1.68 mmol) of 1,2-dihydro- 3-methyl-1-[6-[(2,2,2-trifluoro)ethanesulfonamido]hexan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one in 15 ml of methanol was added 0.17 ml of conc. HCl, then the solvent was distilled off. To the residue were added acetone and ether. The resulting crystals were washed with ether and dried to give 718 mg of the desired compound (94.1%, colorless crystals), m.p.141.0-143.0° C.

Workup

  1. distillationthe solvent was distilled off
  2. additionTo the residue were added acetone and ether
  3. washThe resulting crystals were washed with ether
  4. customdried

Sources & evidence

ORD record
ord-facdb1b7b6034575ba3e861e5f0d131f
Source dataset
uspto-grants-1999_09
Patent number
US05958942

Reaction notes

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