O-Phenylenediamine → HCID 22156921, compound

HRID 1073805Notes

Reaction equation

HRID 1073805 reaction equation
Cl.[CH3:2][N:3]([CH3:10])[CH2:4][CH2:5][CH2:6][C:7](O)=O.[C:11]1([NH2:18])[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH2:17]>O>[CH3:2][N:3]([CH3:10])[CH2:4][CH2:5][CH2:6][C:7]1[NH:17][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[N:18]=1

Participants

4

Reactant 2

HCID 7243O-PhenylenediamineHCID 126916404-(Dimethylamino)butyric acid hydrochloride

Product 1

HCID 22156921HCID 22156921, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Grams 10 4-dimethylaminobutyric acid hydrochloride are heated up till melting together with 6.45 g o-phenylendiamine then it is allowed to cool and 150 ml water are added thereto. The solution is washed with dichloromethane, made alkaline and extracted with dichloromethane. The extracts are collected together, filtered on charcoal, made anhydrous on sodium sulphate and evaporated to dryness. A thick oily reddish residue is obtained, which is triturated with 200 ml diethyl ether to give 5.8 g 2-(3-dimethylaminopropyl)benzimidazole melting at 117°-119° C.

Workup

  1. temperatureto cool
  2. washThe solution is washed with dichloromethane
  3. extractionextracted with dichloromethane
  4. customThe extracts are collected together
  5. filtrationfiltered on charcoal
  6. customevaporated to dryness
  7. customA thick oily reddish residue is obtained
  8. customwhich is triturated with 200 ml diethyl ether

Sources & evidence

ORD record
ord-efe060dfc8f14f78b14f317321337225
Source dataset
uspto-grants-1990_11
Patent number
US04971980

Reaction notes

Loading…