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

HRID 361407

反応式

HRID 361407 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-403951847e7645e5a6556663da6b4841
出典データセット
uspto-grants-1999_02
特許番号
US05866580

関連ノート

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