Hydroxyamine hydrochloride → 3-Cyano-5-cyclobutyl-4-methoxybenzoic acid

HRID 385051노트

반응식

HRID 385051 반응식
[CH:1]1([C:5]2[CH:6]=[C:7]([CH:11]=[C:12]([CH:16]=O)[C:13]=2[O:14][CH3:15])[C:8]([OH:10])=[O:9])[CH2:4][CH2:3][CH2:2]1.Cl.[NH2:19]O>C(O)=O>[C:16]([C:12]1[CH:11]=[C:7]([CH:6]=[C:5]([CH:1]2[CH2:4][CH2:3][CH2:2]2)[C:13]=1[O:14][CH3:15])[C:8]([OH:10])=[O:9])#[N:19]

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 866681583-Cyclobutyl-5-formyl-4-methoxybenzoic acid

생성물 1

HCID 681083433-Cyano-5-cyclobutyl-4-methoxybenzoic acid수율 89.4%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

3-cyclobutyl-5-formyl-4-methoxybenzoic acid (458 mg) was dissolved in formic acid (2.5 mL), and hydroxylamine hydrochloride (163 mg) was added to the solution, and then the mixture was refluxed for 19 hours. The solvent was distilled off under reduced pressure and water 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 (404 mg) as a brown solid.

후처리

  1. temperaturethe mixture was refluxed for 19 hours
  2. distillationThe solvent was distilled off under reduced pressure and water
  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-8583e1039c9a49308f8b2e748e4f605a
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367843B2

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