Trifluoroacetic anhydride → HCID 58478791, 화합물

HRID 1254084노트

반응식

HRID 1254084 반응식
[CH3:1][C:2]1[N+:7]([O-])=[C:6]2[CH2:9][O:10][C:11](=[O:12])[C:5]2=[CH:4][CH:3]=1.FC(F)(F)C(OC(=O)C(F)(F)F)=[O:16]>ClCCl>[OH:16][CH2:1][C:2]1[N:7]=[C:6]2[CH2:9][O:10][C:11](=[O:12])[C:5]2=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 67314368HCID 67314368, 화합물

생성물 1

HCID 58478791HCID 58478791, 화합물수율 57.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-methyl-7H-furo[3,4-b]pyridin-5-one N-oxide (122 mg, 0.74 mmol) in dichloromethane (2 mL) is heated at reflux. Trifluoroacetic anhydride (1.5 mL, 10 mmol) is added dropwise and heating is continued for approximately 30 min. The reaction mixture is cooled and concentrated. The residue is treated with methanol (3 mL) and triethylamine (2 mL) and stirred until no starting material remained. The reaction mixture is concentrated and the residue is purified by chromatography (silica gel). The product containing fractions are concentrated to give the title compound (70 mg, 42%).

후처리

  1. temperatureat reflux
  2. temperatureheating
  3. temperatureThe reaction mixture is cooled
  4. concentrationconcentrated
  5. additionThe residue is treated with methanol (3 mL) and triethylamine (2 mL)
  6. concentrationThe reaction mixture is concentrated
  7. customthe residue is purified by chromatography (silica gel)
  8. additionThe product containing fractions
  9. concentrationare concentrated

출처 및 근거

ORD 기록
ord-c75cbeaab6d2411988deacb2381c273b
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455535B2

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