Trifluoroacetic anhydride → HCID 58478791, 화합물

HRID 1011338노트

반응식

HRID 1011338 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-e28a1d04c6804074a0036250ab475997
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977351B2

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