p-Toluenesulfonic acid → HCID 178498584、化合物

HRID 1032582ノート

反応式

HRID 1032582 の反応式
[OH:1][C:2]1[N:7]2[N:8]=[C:9]([CH2:11][OH:12])[N:10]=[C:6]2[N:5]=[C:4]([C:13]([O:15][CH3:16])=[O:14])[CH:3]=1.CN(C=O)C.[C:22](OC(=O)C)(=[O:24])[CH3:23].C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[C:22]([O:12][CH2:11][C:9]1[N:10]=[C:6]2[N:5]=[C:4]([C:13]([O:15][CH3:16])=[O:14])[CH:3]=[C:2]([OH:1])[N:7]2[N:8]=1)(=[O:24])[CH3:23]

参加物

6

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 178498586HCID 178498586、化合物

生成物 1

HCID 178498584HCID 178498584、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

A mixture of 25.7 g of 7-hydroxy-2-hydroxymethyl-5-methoxycarbonyl-s-triazolo[1,5-a]pyrimidine, 200 of DMF, 47 ml of acetic anhydride and 1 g of p-toluenesulfonic acid was stirred at 60° C. for 24 hours. The reaction mixture was condensed and 100 ml of methanol was added to the crystals precipitated residue, and the mixture was stirred. Then, crystals were collected by filtration, washed with methanol and dried to obtain 8.9 g of the title compound.

後処理

  1. additionwas added to the crystals
  2. customprecipitated residue
  3. stirringthe mixture was stirred
  4. filtrationThen, crystals were collected by filtration
  5. washwashed with methanol
  6. customdried

出典と根拠

ORDレコード
ord-6ec77b0207f6434da0834788576b5971
出典データセット
uspto-grants-1990_09
特許番号
US04958019

反応ノート

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