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

HRID 33376노트

반응식

HRID 33376 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

20 g (71 mmol) 7-acetyl-5-benzyloxy-3H-benzoxazol-2-one and 8 g (72 mmol) selenium dioxide are refluxed for 8 hours in the presence of activated charcoal in 100 mL dioxane and 3.1 mL water. 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 precipitated on cooling is suction filtered after 3 hours and washed with ethanol and diethyl ether.

후처리

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

출처 및 근거

ORD 기록
ord-84c88a4e7743428886811c5169da4e36
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429583B2

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