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Sodium borohydride → HCID 178432391, 화합물

HRID 1032214
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HRID 1032214 반응식
[OH:1][C:2]1[N:7]2[N:8]=[C:9]([CH3:11])[N:10]=[C:6]2[N:5]=[C:4]([C:12](OC)=[O:13])[CH:3]=1.[BH4-].[Na+]>C(O)C>[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 178498583HCID 178498583, 화합물

생성물 1

HCID 178432391HCID 178432391, 화합물수율 100.1%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

In 4 liters of ethanol was suspended 45.4 g of 7-hydroxy-5-methoxycarbonyl-2-methyl-s-triazolo[1,5-a]pyrimidine and 37.83 g of sodium borohydride was added little by little thereto, and the mixture was then stirred at room temperature for 3 hours. A residue obtained by removing ethanol was dissolved in 2 liters of water, and 500 ml of Amberlite IRC-50 (H+) (trade name) was added thereto and stirred. Subsequently, the mixture was filtered and after removing water from the filtrate, 500 ml of methanol was added to the filtrate and the mixture was stirred. Then, methanol was removed from the mixture to obtain a residue. These procedures were repeated three times. Then, 500 ml of ethanol was added to the residue and the mixture was condensed. Precipitated crystals were collected by filtration, washed with ethanol and dried to obtain 39.35 g of the title compound.

후처리

  1. additionwas added little by little thereto, and the mixture
  2. customA residue obtained
  3. customby removing ethanol
  4. dissolutionwas dissolved in 2 liters of water
  5. addition500 ml of Amberlite IRC-50 (H+) (trade name) was added
  6. stirringstirred
  7. filtrationSubsequently, the mixture was filtered
  8. customafter removing water from the filtrate, 500 ml of methanol
  9. additionwas added to the filtrate
  10. stirringthe mixture was stirred
  11. customThen, methanol was removed from the mixture
  12. customto obtain a residue
  13. customcondensed
  14. customPrecipitated crystals
  15. filtrationwere collected by filtration
  16. washwashed with ethanol
  17. customdried

출처 및 근거

ORD 기록
ord-eb7cdbbcee95477a8fff416315d5b8f5
출처 데이터셋
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04956462

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