Sodium borohydride → HCID 178519774、化合物

HRID 1032221ノート

反応式

HRID 1032221 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](OC)=[O:14])[CH:3]=1.[BH4-].[Na+]>C(O)C>[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]([CH2:13][OH:14])[CH:3]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 178498586HCID 178498586、化合物

生成物 1

HCID 178519774HCID 178519774、化合物収率 91.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 4 liters of ethanol was suspended 48.94 g of 7-hydroxy-2-hydroxymethyl-5-methoxycarbonyl-s-triazolo[1,5-a]pyrimidine, and 33 g of sodium borohydride was added little by little thereto and then the mixture was stirred at room temperature for 3 hours and then refluxed for 4 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 crystal was collected by filtration, washed with ethanol and dried to obtain 39.35 g of the title compound.

後処理

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

出典と根拠

ORDレコード
ord-864400f22b1e4ec38dd6b3b691150c12
出典データセット
uspto-grants-1990_09
特許番号
US04956462

反応ノート

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