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 1068732Notes

Reaction equation

HRID 1068732 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-6dcc26cc50c642b7aadbaf99c22ece12
Source dataset
uspto-grants-2001_06
Patent number
US06251905B1

Reaction notes

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