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

HRID 385144노트

반응식

HRID 385144 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 681091153-Cyano-4-methoxy-5-trifluoromethoxybenzoic acid수율 95.2%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ee7ce77016534c12a0ed65ed14c712b4
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367843B2

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