Acetic Acid → HCID 178440143, compound

HRID 265109Notes

Reaction equation

HRID 265109 reaction equation
[OH:1][CH:2]([C:7]1[N:8]=[C:9]([CH2:51][CH2:52][CH3:53])[N:10]([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)[C:11]=1[C:12]#[N:13])[C:3]([CH3:6])([CH3:5])[CH3:4].C(O)(=O)C>O>[OH:1][CH:2]([C:7]1[N:8]=[C:9]([CH2:51][CH2:52][CH3:53])[N:10]([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[NH:31][N:30]=[N:29][N:28]=3)=[CH:17][CH:16]=2)[C:11]=1[C:12]#[N:13])[C:3]([CH3:6])([CH3:4])[CH3:5]

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 19036248HCID 19036248, compound

Product 1

HCID 178440143HCID 178440143, compoundYield 99.3%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
60 °C

Procedure

A suspension of 1.65 g of 4-(1-hydroxy-2,2-dimethylpropyl)-2-propyl-1-{4-[2-(trityltetrazol-5-yl)phenyl]-phenyl}methylimidazole-5-carbonitrile [prepared as described in step (b) above] in 24 ml of 75% v/v aqueous acetic acid was stirred at 60° C. for 2 hours. At the end of this time, 6 ml of water was added to the reaction mixture, which was then cooled with ice. The trityl alcohol which precipitated was removed by filtration, and the filtrate was concentrated by evaporation under reduced pressure, to give 1.07 g of the title compound as a glass.

Workup

  1. temperaturewas then cooled with ice
  2. customThe trityl alcohol which precipitated
  3. customwas removed by filtration
  4. concentrationthe filtrate was concentrated by evaporation under reduced pressure

Sources & evidence

ORD record
ord-4afbaebd24394651b151e1a052829962
Source dataset
uspto-grants-1997_07
Patent number
US05646171

Reaction notes

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