Acetic Acid → HCID 178475878, compound

HRID 704505Notes

Reaction equation

HRID 704505 reaction equation
[OH:1][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=[C:4]([CH2:12][OH:13])[CH:3]=1.CN(C=O)C.[C:19](O)(=[O:21])[CH3:20].C1(C)C=CC(S(O)(=O)=O)=CC=1>CCOCC.C(O)(C)C>[C:19]([O:13][CH2:12][C:4]1[CH:3]=[C:2]([OH:1])[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=1)(=[O:21])[CH3:20]

Participants

7

Reactant 4

HCID 176Acetic AcidHCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 178432391HCID 178432391, compound

Product 1

HCID 178475878HCID 178475878, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 3776IsopropanolSolvent

Conditions

Temperature
50 °C

Procedure

A mixture of 33.06 g of 7-hydroxy-5-hydroxymethyl-2-methyl-s-triazolo[1,5-a]pyrimidine, 500 ml of DMF, 86 ml of anhydrous acetic acid and 1.5 g of p-toluenesulfonic acid was stirred in a bath at 50 ° C. for 6 hours. To an oily isopropanol to dissolve therein, and the solution was dropwise in 4 liters of ether. Precipitates were collected by filtration and dried to obtain 38.08 g of the compound.

Workup

  1. customPrecipitates
  2. filtrationwere collected by filtration
  3. customdried

Sources & evidence

ORD record
ord-b08ce1cfa1334cc4946ef42ab590d8bf
Source dataset
uspto-grants-1991_01
Patent number
US04987129

Reaction notes

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