Methanol → HCID 178437100, compound

HRID 2260056Notes

Reaction equation

HRID 2260056 reaction equation
[CH2:1]([C:3]1[C:10]2[N:6]([N:7]=[C:8]([CH:11]([CH3:13])[CH3:12])[N:9]=2)[N:5]([CH2:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[N:31](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[CH:4]=1)[CH3:2].CO>C(O)(=O)C>[CH2:1]([C:3]1[C:10]2[N:6]([N:7]=[C:8]([CH:11]([CH3:13])[CH3:12])[N:9]=2)[N:5]([CH2:14][C:15]2[CH:16]=[CH:17][C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[C:27]3[NH:28][N:29]=[N:30][N:31]=3)=[CH:19][CH:20]=2)[CH:4]=1)[CH3:2]

Participants

4

Reactant 2

HCID 887MethanolHCID 10604331HCID 10604331, compound

Product 1

HCID 178437100HCID 178437100, compoundYield 95.4%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture consisting of 2.38 g of 7-ethyl-2-isopropyl-5-[[2'-(N-triphenylmethyl-tetrazol-5-yl)biphenyl-4-yl]methyl]-5H-pyrazolo[1,5-b][1,2,4]triazole, 90 ml of methanol and 10 ml of acetic acid was heated under reflux for 2 hours. After removing the solvent by distillation under a reduced pressure, the thus obtained residue was subjected to silica gel column chromatography. Elution with methanol-chloroform (1:9, v/v) gave 1.43 g of 7-ethyl-2-isopropyl-5-[[2'-(tetrazol-5-yl)biphenyl-4-yl]methyl]-5H-pyrazolo[1,5-b][1,2,4]triazole in the form of colorless amorphous foamy material.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. customAfter removing the solvent
  4. distillationby distillation under a reduced pressure
  5. washElution with methanol-chloroform (1:9, v/v)

Sources & evidence

ORD record
ord-8e6517a4d4e34fcca18729025a244a85
Source dataset
uspto-grants-1995_12
Patent number
US05475114

Reaction notes

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