ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methane → 5-benzyloxy-8-(2-ethoxy-2-hydroxy-acetyl)-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one

HRID 969453
ノート
印刷プレビュー

反応式

HRID 969453 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[C:7]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[CH:6][CH:5]=1)(=[O:3])[CH3:2].[Se](=O)=O.C.[OH2:29].[O:30]1CCO[CH2:32][CH2:31]1>>[CH2:18]([O:17][C:7]1[C:8]2[NH:9][C:10](=[O:16])[C:11]([CH3:15])([CH3:14])[O:12][C:13]=2[C:4]([C:1](=[O:3])[CH:2]([O:30][CH2:31][CH3:32])[OH:29])=[CH:5][CH:6]=1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 297MethaneHCID 962WaterHCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 694623038-acetyl-5-benzyloxy-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one

生成物 1

HCID 590172615-benzyloxy-8-(2-ethoxy-2-hydroxy-acetyl)-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one

実験手順

9.6 g (30 mmol) 8-acetyl-5-benzyloxy-2,2-dimethyl-4H-benzo[1,4]oxazin-3-one, 3.3 g (30 mmol) selenium dioxide and activated charcoal are stirred for 7 hours in 90 mL dioxane and 2 mL water at reflux temperature. The solid is suction filtered, the filtrate is evaporated down and the residue is refluxed for 30 minutes in 100 ml of ethanol. The solvent is distilled off and the residue is dissolved in 125 mL ethyl acetate. It is extracted successively with potassium carbonate solution and water, dried with sodium sulphate and evaporated down. The oil remaining (10.1 g) is further reacted directly.

後処理

  1. filtrationfiltered
  2. customthe filtrate is evaporated down
  3. temperaturethe residue is refluxed for 30 minutes in 100 ml of ethanol
  4. distillationThe solvent is distilled off
  5. dissolutionthe residue is dissolved in 125 mL ethyl acetate
  6. extractionIt is extracted successively with potassium carbonate solution and water
  7. dry with materialdried with sodium sulphate
  8. customevaporated down
  9. customis further reacted directly

出典と根拠

ORDレコード
ord-024ca60da1444369a28f002d212879ce
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07307076B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート