Hydrochloric Acid → N-[3,5-Bis(trifluoromethyl)phenyl]-5-ethynyl-2-hydroxybenzamide

HRID 421054노트

반응식

HRID 421054 반응식
[F:1][C:2]([F:30])([F:29])[C:3]1[CH:4]=[C:5]([NH:13][C:14](=[O:28])[C:15]2[CH:20]=[C:19]([C:21]#[C:22][Si](C)(C)C)[CH:18]=[CH:17][C:16]=2[OH:27])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[OH-].[Na+].Cl>CO>[F:1][C:2]([F:29])([F:30])[C:3]1[CH:4]=[C:5]([NH:13][C:14](=[O:28])[C:15]2[CH:20]=[C:19]([C:21]#[CH:22])[CH:18]=[CH:17][C:16]=2[OH:27])[CH:6]=[C:7]([C:9]([F:10])([F:11])[F:12])[CH:8]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 10343463N-[3,5-Bis(trifluoromethyl)phenyl]-2-hydroxy-5-[(trimethylsilyl)ethynyl]benzamide

생성물 1

HCID 11773173N-[3,5-Bis(trifluoromethyl)phenyl]-5-ethynyl-2-hydroxybenzamide수율 35.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

N-[3,5-Bis(trifluoromethyl)phenyl]-2-hydroxy-5-[(trimethylsilyl)ethynyl]benzamide (233 mg, 0.5 mmol) was dissolved in methanol (1 mL). 2 N sodium hydroxide (1 mL) was added, and the mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into 2 N hydrochloric acid and extracted with ethyl acetate. After the ethyl acetate layer was washed with water and brine one after another, dried over anhydrous magnesium sulfate, the solvent was evaporated under reduced pressure. The obtained residue was crystallized from ethanol-water to give the title compound (67 mg, 35.9%) as a light gray crystal.

후처리

  1. extractionextracted with ethyl acetate
  2. washAfter the ethyl acetate layer was washed with water and brine one after another,
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe obtained residue was crystallized from ethanol-water

출처 및 근거

ORD 기록
ord-dd96188744524987ad3aa14ed86abe48
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08097759B2

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