Trifluoroacetic anhydride → HCID 58478791、化合物

HRID 1011338ノート

反応式

HRID 1011338 の反応式
[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

参加物

4

反応物 2

HCID 9845Trifluoroacetic anhydrideHCID 67314368HCID 67314368、化合物

生成物 1

HCID 58478791HCID 58478791、化合物収率 57.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-e28a1d04c6804074a0036250ab475997
出典データセット
uspto-grants-2011_07
特許番号
US07977351B2

反応ノート

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