Hydrochloric Acid → HCID 70213121, compound

HRID 619450Notes

Reaction equation

HRID 619450 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:22])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][S:18]([CH3:21])(=[O:20])=[O:19].[ClH:23]>CO>[ClH:23].[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:22])[N:8]3[CH2:13][CH2:14][CH2:15][CH2:16][NH:17][S:18]([CH3:21])(=[O:19])=[O:20]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21190079HCID 21190079, compound

Product 1

HCID 70213121HCID 70213121, compoundYield 99.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a suspension of 500 mg (1.55 mmol) of 1,2-dihydro-3-methyl-1-[4-(methanesulfonamido)butan-1-yl]-1,4,7b-triazacyclopent[cd]inden-2-one in 20 ml of methanol was added 0.17 ml of conc. HCl. The solvent was then distilled off. The residue was washed with ether to give 555 mg of the desired compound (99.6%, colorless solid), m.p.166.0-167.0° C. NMR(200 MHz,DMSO-d6) δ: 1.53(2H,m), 1.82(2H,m), 2.79(3H,s), 2.86(3H,s), 2.96(2H,m), 4.09(2H,t,J=6.8 Hz), 7.00(1H,br), 7.56(1H,d,J=7.6 Hz), 7.76(1H,d,J=8.6 Hz), 8.15(1H,dd,J=8.6,7.6 Hz).

Workup

  1. distillationThe solvent was then distilled off
  2. washThe residue was washed with ether

Sources & evidence

ORD record
ord-d99b698ea3984063828ea74289ffd6d7
Source dataset
uspto-grants-1999_09
Patent number
US05958942

Reaction notes

Loading…