Dichloromethane → HCID 23303020, compound

HRID 1489002Notes

Reaction equation

HRID 1489002 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[N:15]3[C:11](=[N:12][C:13]4[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=43)[S:10][N:9]=2)[CH2:4][CH2:3]1.[Cl:20]CCl>Cl>[ClH:20].[ClH:20].[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[N:15]3[C:11](=[N:12][C:13]4[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=43)[S:10][N:9]=2)[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 6344DichloromethaneHCID 10221162HCID 10221162, compound

Product 1

HCID 23303020HCID 23303020, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

To a clear solution of 3-(4-methyl-1-piperazinyl)-1,2,4-thiadiazolo[4,5-a]benzimidazole (6.07 g, 22.21 mmol) in 100 ml of dichloromethane, hydrogen chloride gas was bubbled through for 40 min. The solution became turbid with time. The suspension was filtered and dried under vacuum to give the title compound as a fine white powder 7.60 g (99%). mp 252° C. (dec); 1H NMR (DMSO-d6 & D2O) δ7.85 (d, 2H), 7.60 (t, 1H), 7.51 (t, 1H), 3.86 (m, 2H), 3.56 (m, 6H), 2.91 (s, 3H) ppm; 13C NMR (DMSO-d6 & D2O) δ164.39, 148.80, 144.27, 126.92, 126.12, 123.41, 117.08, 113.20, 51.19, 45.87, 42.32 ppm; IR (KBr) ν3420, 1606, 1571, 1475, 1461, 1225, 981, 761 cm-1.

Workup

  1. filtrationThe suspension was filtered
  2. customdried under vacuum

Sources & evidence

ORD record
ord-e106ea7d237a4740bc7d8e9d393cba13
Source dataset
uspto-grants-1997_10
Patent number
US05677302

Reaction notes

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