Stannous chloride dihydrate → HCID 178432277, compound

HRID 513865Notes

Reaction equation

HRID 513865 reaction equation
Cl.[NH2:2][C:3]1[CH:12]=[CH:11][C:6]2[NH:7][C:8]([CH3:10])=[N:9][C:5]=2[CH:4]=1.[N:13]([O-])=O.[Na+].O.O.[Sn](Cl)Cl>Cl>[CH3:10][C:8]1[NH:7][C:6]2[CH:11]=[CH:12][C:3]([NH:2][NH2:13])=[CH:4][C:5]=2[N:9]=1

Participants

5

Reactant 3

HCID 61436Stannous chloride dihydrateHCID 23668193Sodium NitriteHCID 178432268HCID 178432268, compound

Product 1

HCID 178432277HCID 178432277, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent2×

Conditions

Temperature
0 °C

Procedure

5-Amino-2-methyl-1H-benzimidazol hydrochloride (16.51 g) was dissolved in concentrated hydrochloric acid (200 ml), and this was cooled to 0° C. An aqueous solution (15 ml) of sodium nitrite (7.59 g) was added dropwise thereto at 0° C. over 20 minutes. This was stirred for 20 minutes. Then, a concentrated hydrochloric acid solution (20 ml) of tin (II) chloride dihydrate (55.7 g) was added dropwise thereto at 0° C. over one hour, and then this was stirred for 30 minutes. The precipitated solid was collected by filtration, and washed with water, and dried. Thus, crude (2-methyl-1H-benzimidazol-5-yl)-hydrazine dihydrochlide was obtained.

Workup

  1. waitat 0° C. over one hour
  2. stirringthis was stirred for 30 minutes
  3. filtrationThe precipitated solid was collected by filtration
  4. washwashed with water
  5. customdried

Sources & evidence

ORD record
ord-c853c5d3d9ca402fbbda36a1dca81d3b
Source dataset
uspto-grants-2015_08
Patent number
US09102692B2

Reaction notes

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