p-Toluenesulfonic acid → HCID 178498584, 화합물

HRID 1032582노트

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HRID 1032582 반응식
[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]

참가 물질

6

반응물 4

HCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 7918Acetic AnhydrideHCID 178498586HCID 178498586, 화합물

생성물 1

HCID 178498584HCID 178498584, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6ec77b0207f6434da0834788576b5971
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04958019

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