Methane → 5-(Benzyloxy)-7-[ethoxy(hydroxy)acetyl]-1,3-benzoxazol-2(3H)-one

HRID 969447ノート

反応式

HRID 969447 の反応式
[C:1]([C:4]1[C:12]2[O:11][C:10](=[O:13])[NH:9][C:8]=2[CH:7]=[C:6]([O:14][CH2:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH:5]=1)(=[O:3])[CH3:2].[Se](=O)=[O:23].C.[O:26]1CCO[CH2:28][CH2:27]1>O>[CH2:15]([O:14][C:6]1[CH:5]=[C:4]([C:1](=[O:3])[CH:2]([O:26][CH2:27][CH3:28])[OH:23])[C:12]2[O:11][C:10](=[O:13])[NH:9][C:8]=2[CH:7]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

6

反応物 4

HCID 297MethaneHCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 210728587-Acetyl-5-(benzyloxy)-1,3-benzoxazol-2(3H)-one

生成物 1

HCID 210728515-(Benzyloxy)-7-[ethoxy(hydroxy)acetyl]-1,3-benzoxazol-2(3H)-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

20 g (71 mmol) 7-acetyl-5-benzyloxy-3H-benzoxazol-2-one and 8 g (72 mmol) selenium dioxide are stirred in the presence of activated charcoal in 100 mL dioxane and 3.1 mL water for 8 hours at reflux temperature. The solid is filtered off, the solvent is distilled off and the residue is combined with 50 mL ethanol. The mixture is refluxed for 15 minutes and then filtered through activated charcoal. The solid that precipitates on cooling is suction filtered for 3 hours and washed with ethanol and diethyl ether.

後処理

  1. temperatureat reflux temperature
  2. filtrationThe solid is filtered off
  3. distillationthe solvent is distilled off
  4. temperatureThe mixture is refluxed for 15 minutes
  5. filtrationfiltered through activated charcoal
  6. customThe solid that precipitates
  7. temperatureon cooling
  8. filtrationis suction filtered for 3 hours
  9. washwashed with ethanol and diethyl ether

出典と根拠

ORDレコード
ord-1dc5008e3017447abec781a37859da63
出典データセット
uspto-grants-2007_12
特許番号
US07307076B2

反応ノート

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