Hydrogen Peroxide → HCID 178507181, 화합물

HRID 929321노트

반응식

HRID 929321 반응식
[C@@H:1]1([N:10]2[C:19]3[N:18]=[CH:17][N:16]=[C:14]([NH2:15])[C:13]=3[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3].C1N=C(N)C2N=CN([C@@H]3[O:34][C@H](CO)[C@@H](O)[C@@H]3O)C=2N=1.O.OO>C(O)(=O)C.[C].[Pd]>[C@@H:1]1([N:10]2[C:19]3[C:13](=[C:14]([N+:16]([O-:34])=[CH:17][N:18]=3)[NH2:15])[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3]

참가 물질

6

반응물 3

HCID 784Hydrogen Peroxide2회HCID 323269-Pentofuranosyl-9H-purin-6-amine--water (1/1)HCID 60961Adenosine

생성물 1

HCID 178507181HCID 178507181, 화합물

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 176Acetic Acid용매

실험 절차

Twenty grams of adenosine with a product code of A9251-25G, commercialized by Sigma-Aldrich Japan K.K., Tokyo, Japan, was dispersed in one liter of acetic acid and admixed with 100 mL of 30% hydrogen peroxide solution, followed by stirring the resulting mixture at ambient temperature for five days. An excessive amount of the remaining hydrogen peroxide was decomposed by the addition of five grams of 5% palladium carbon, commercialized by Kawaken Fine Chemicals Co., Ltd., Tokyo, Japan, followed by filtering the mixture to remove the palladium carbon, drying the resulting solution in vacuo, adding ethanol to the dried product to disperse the formed crystals, and filtering the resulting mixture to obtain crude crystals of adenosine N1-oxide. Eight grams of adenosine N1-oxide with a purity of 99.5% was obtained by dissolving the crude crystals in ethanol by heating, filtering the resulting solution, ice-chilling the filtrate to effect recrystallization, and repeating these steps twice.

후처리

  1. filtrationby filtering the mixture
  2. customto remove the palladium carbon
  3. customdrying the resulting solution in vacuo
  4. additionadding ethanol to the dried product
  5. additionto disperse the formed crystals
  6. filtrationfiltering the resulting mixture

출처 및 근거

ORD 기록
ord-2b32604384a4425db62ef4c56cd11770
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09295627B2

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