Ethyl orthoformate → Methyl (1,3-benzoxazol-5-yl)acetate

HRID 660277

반응식

HRID 660277 반응식
[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([NH2:12])[CH:6]=1.[CH:14](OCC)(OCC)OCC>O>[CH3:1][O:2][C:3](=[O:13])[CH2:4][C:5]1[CH:10]=[CH:9][C:8]2[O:11][CH:14]=[N:12][C:7]=2[CH:6]=1

참가 물질

4

반응물 2

HCID 31214Ethyl orthoformateHCID 1475136Methyl 2-(3-amino-4-hydroxyphenyl)acetate

생성물 1

HCID 16413026Methyl (1,3-benzoxazol-5-yl)acetate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Methyl-2-(3-amino-4-hydroxyphenyl)acetate (1.39 g, 7.67 mmol) was combined at RT with triethyl orthoformate (10 ml). The reaction mixture was heated to reflux for 12 h and then cooled to RT. Water (70 mL) was added thereto and the reaction mixture was extracted with EA. The combined organic phases were dried over MgSO4 and filtered. The solvent was removed under a vacuum and the residue purified by means of column chromatography (n-hexane/EA=2:1).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 12 h
  3. extractionthe reaction mixture was extracted with EA
  4. dry with materialThe combined organic phases were dried over MgSO4
  5. filtrationfiltered
  6. customThe solvent was removed under a vacuum
  7. customthe residue purified by means of column chromatography (n-hexane/EA=2:1)

출처 및 근거

ORD 기록
ord-6d899332cb7140c3ac23056d1c6960da
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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