Acetic Acid → HCID 178440143, compound

HRID 52970Notes

Reaction equation

HRID 52970 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-dimethyl propyl)-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-6450204ed6c040318bf70c6c9035647e
Source dataset
uspto-grants-1997_04
Patent number
US05616599

Reaction notes

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