Hydroxyamine hydrochloride → 3-Cyano-4-methoxy-5-trifluoromethoxybenzoic acid

HRID 385144ノート

反応式

HRID 385144 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][C:15]([F:18])([F:17])[F:16])[C:11]=1[O:12][CH3:13])[C:6]([OH:8])=[O:7])=O.Cl.[NH2:20]O>C(O)=O>[C:1]([C:3]1[CH:4]=[C:5]([CH:9]=[C:10]([O:14][C:15]([F:18])([F:17])[F:16])[C:11]=1[O:12][CH3:13])[C:6]([OH:8])=[O:7])#[N:20]

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 866681823-Formyl-4-methoxy-5-trifluoromethoxybenzoic acid

生成物 1

HCID 681091153-Cyano-4-methoxy-5-trifluoromethoxybenzoic acid収率 95.2%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

3-formyl-4-methoxy-5-trifluoromethoxybenzoic acid (4.22 g) was dissolved in formic acid (20 mL), and hydroxylamine hydrochloride (1.22 g) was added to the solution, and then the mixture was refluxed for 16 hours. The solvent was distilled off under reduced pressure and 1N hydrochloric acid was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain the title compound (3.97 g) as a brown solid.

後処理

  1. temperaturethe mixture was refluxed for 16 hours
  2. distillationThe solvent was distilled off under reduced pressure and 1N hydrochloric acid
  3. additionwas added
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-ee7ce77016534c12a0ed65ed14c712b4
出典データセット
uspto-grants-2013_02
特許番号
US08367843B2

反応ノート

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