Acetic Anhydride → (2,4-Dihydroxypyrido[3,2-d]pyrimidin-6-yl)methyl acetate

HRID 361407

반응식

HRID 361407 반응식
[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([CH3:12])=[N:11][C:5]=2[C:4](=[O:13])[NH:3]1.C1C=C(Cl)C=[C:16]([C:21]([O:23]O)=[O:22])C=1.C(OC(=O)C)(=O)C>C(O)(=O)C>[C:21]([O:23][CH2:12][C:10]1[CH:9]=[CH:8][C:6]2[NH:7][C:2](=[O:1])[NH:3][C:4](=[O:13])[C:5]=2[N:11]=1)(=[O:22])[CH3:16]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 70297m-Chloroperbenzoic acidHCID 2732402499-96-9

생성물 1

HCID 22281841(2,4-Dihydroxypyrido[3,2-d]pyrimidin-6-yl)methyl acetate수율 66%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

1.77 g of 1 (10 mmol) in 50 ml of glacial acetic acid containing 6.5 g of MCPBA (57-85%) was refluxed for 3 hours. Acetic anhydride (40 ml) was added to the hot reaction mixture and the refluxing was continued for another half an hour. The clear brown solution was evaporated to dryness and the solid was stirred with ether (100 ml) and filtered. The solid was crystallized from ethanol to give 1.55 g (66%) of 2.

후처리

  1. waitthe refluxing was continued for another half an hour
  2. customThe clear brown solution was evaporated to dryness
  3. filtrationfiltered
  4. customThe solid was crystallized from ethanol

출처 및 근거

ORD 기록
ord-403951847e7645e5a6556663da6b4841
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866580

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