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Methane → 6-benzyloxy-8-(2-ethoxy-2-hydroxy-acetyl)-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one

HRID 1372902
ノート
印刷プレビュー

反応式

HRID 1372902 の反応式
[C:1]([C:4]1[C:13]2[O:12][C:11]([CH3:15])([CH3:14])[C:10](=[O:16])[NH:9][C:8]=2[CH:7]=[C:6]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:5]=1)(=[O:3])[CH3:2].[Se](=O)=[O:26].C.[O:29]1CCO[CH2:31][CH2:30]1>O>[CH2:18]([O:17][C:6]1[CH:5]=[C:4]([C:1](=[O:3])[CH:2]([O:29][CH2:30][CH3:31])[OH:26])[C:13]2[O:12][C:11]([CH3:15])([CH3:14])[C:10](=[O:16])[NH:9][C:8]=2[CH:7]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 297MethaneHCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 21072863HCID 21072863、化合物

生成物 1

HCID 210728546-benzyloxy-8-(2-ethoxy-2-hydroxy-acetyl)-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-18 °C

実験手順

50.12 g (154 mmol) 8-acetyl-6-benzyloxy-2,2-dimethyl-benzo[1,4]oxazin-3-one are reacted with selenium dioxide as oxidising agent and activated charcoal in refluxing dioxane and some water. After cooling, the solid is filtered off and washed with dioxane. The filtrate is evaporated down and the residue is dissolved in 550 mL ethanol and refluxed for 30 minutes. It is filtered and the mother liquor is cooled to −18° C., during which time a solid is precipitated which is suction filtered. After recrystallisation from ethanol the product is obtained in the form of a beige solid. Yield: 8.95 g (15%).

後処理

  1. temperatureAfter cooling
  2. filtrationthe solid is filtered off
  3. washwashed with dioxane
  4. customThe filtrate is evaporated down
  5. dissolutionthe residue is dissolved in 550 mL ethanol
  6. temperaturerefluxed for 30 minutes
  7. filtrationIt is filtered
  8. customis precipitated which
  9. filtrationfiltered
  10. customAfter recrystallisation from ethanol the product
  11. customis obtained in the form of a beige solid

出典と根拠

ORDレコード
ord-29c15422cf4047f4be2ba901555b263e
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07160882B2

反応ノート

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