Methylamine → HCID 22405431, compound

HRID 440837Notes

Reaction equation

HRID 440837 reaction equation
[CH2:1]([C:4]1[N:8]([CH2:9][C:10]2[CH:15]=[CH:14][C:13]([C:16]3[C:17]([C:22]([O:24][CH3:25])=[O:23])=[CH:18][CH:19]=[CH:20][CH:21]=3)=[CH:12][CH:11]=2)[C:7]2[CH:26]=[C:27]([N:31]3C(=O)C4=CC=CC=C4C3=O)[CH:28]=[C:29]([Cl:30])[C:6]=2[N:5]=1)[CH2:2][CH3:3].CN>C(O)C>[CH2:1]([C:4]1[N:8]([CH2:9][C:10]2[CH:11]=[CH:12][C:13]([C:16]3[C:17]([C:22]([O:24][CH3:25])=[O:23])=[CH:18][CH:19]=[CH:20][CH:21]=3)=[CH:14][CH:15]=2)[C:7]2[CH:26]=[C:27]([NH2:31])[CH:28]=[C:29]([Cl:30])[C:6]=2[N:5]=1)[CH2:2][CH3:3]

Participants

4

Reactant 2

HCID 6329MethylamineHCID 22405442HCID 22405442, compound

Product 1

HCID 22405431HCID 22405431, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

2.05 g of methyl 4'-[(2-n-propyl-4-chloro-6-phthalimido-1H -benzimidazol-1-yl)-methyl]-biphenyl-2-carboxylate are dissolved in 125 ml of ethanol and mixed with 5 ml of a 40% aqueous methylamine solution. The reaction mixture is stirred for 3 hours at ambient temperature and then stirred into saline solution. After extracting 3 times with ethyl acetate the combined organic phases are dried over sodium sulphate and evaporated down. The residue is stirred with petroleum ether/ether (1:4) for 24 hours, the solids formed are suction filtered and dried.

Workup

  1. stirringstirred into saline solution
  2. extractionAfter extracting 3 times with ethyl acetate the combined organic phases
  3. dry with materialare dried over sodium sulphate
  4. customevaporated down
  5. stirringThe residue is stirred with petroleum ether/ether (1:4) for 24 hours
  6. customthe solids formed
  7. filtrationfiltered
  8. customdried

Sources & evidence

ORD record
ord-d08b6773ac074c61bb2b78adbd3f3a58
Source dataset
uspto-grants-1996_05
Patent number
US05521177

Reaction notes

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