Dichloromethane → HCID 23303020, compound

HRID 2289606Notes

Reaction equation

HRID 2289606 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 ) δ 7.85 (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) δ 164.39, 148.80, 144.27, 126.92, 126.12, 123.41, 117.08, 113.20, 51.19, 45.87, 42.32 ppm; IR (KBr) ν 3420, 1606, 1571, 1475, 1461, 1225, 981, 761 cm-1.

Workup

  1. filtrationThe suspension was filtered
  2. customdried under vacuum

Sources & evidence

ORD record
ord-ff2b6c6ded004a3f96a8dc18889d8cb5
Source dataset
uspto-grants-2000_07
Patent number
US06093738

Reaction notes

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