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p-Toluenesulfonic acid → HCID 178475878, 화합물

HRID 1032586
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HRID 1032586 반응식
[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([CH:17]=[O:18])C.[C:19]1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)(=O)C>[C:17]([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:18])[CH3:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6101p-Toluenesulfonic acidHCID 6228DimethylformamideHCID 178432391HCID 178432391, 화합물

생성물 1

HCID 178475878HCID 178475878, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
50 °C

실험 절차

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 residue obtained by removing DMF was added 300 ml of isopropanol to dissolve therein, and the solution was added dropwise in 4 liters of ether. Precipitates were collected by filtration and dried to obtain 38.08 g of the title compound.

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후처리

  1. customTo an oily residue obtained
  2. customby removing DMF
  3. additionwas added 300 ml of isopropanol
  4. dissolutionto dissolve
  5. additionthe solution was added dropwise in 4 liters of ether
  6. customPrecipitates
  7. filtrationwere collected by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-43d8b391ac514f888191b7dbf657510b
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04958019

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