HCID 67059672, 화합물 → HCID 67059665, 화합물

HRID 1807772노트

반응식

HRID 1807772 반응식
C([NH:8][C:9]1[C:18]([F:19])=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[C:11]([Br:20])[CH:10]=1)C1C=CC=CC=1.[H][H]>C(O)(=O)C.[Pd].CO>[NH2:8][C:9]1[C:18]([F:19])=[CH:17][C:12]([C:13]([O:15][CH3:16])=[O:14])=[C:11]([Br:20])[CH:10]=1

참가 물질

6

반응물 2

HCID 67059672HCID 67059672, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 67059665HCID 67059665, 화합물수율 73.8%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 887Methanol용매

실험 절차

A suspension of the methyl 4-(benzylamino)-2-bromo-5-fluorobenzoate (2.4 g, 7.10 mmol) in acetic acid was treated with 10% palladium on charcoal (250 mg) and stirred at room temperature under 2 bar hydrogen for 18 hours. The reaction mixture was then diluted with methanol, filtered through celite and evaporated to low volume. The residue was suspended in water (50 mL) and basified with 5% sodium carbonate solution then was extracted with ethyl acetate (2×). The combined organic phases were dried (sodium sulfate) and evaporated to a sandy solid. This crude solid was dissolved in the methanol and passed down an SCX cartridge. Evaporation of the methanol eluents gave the title compound (1.3 g).

후처리

  1. filtrationfiltered through celite
  2. customevaporated to low volume
  3. extractionthen was extracted with ethyl acetate (2×)
  4. dry with materialThe combined organic phases were dried (sodium sulfate)
  5. customevaporated to a sandy solid
  6. dissolutionThis crude solid was dissolved in the methanol
  7. customEvaporation of the methanol eluents

출처 및 근거

ORD 기록
ord-d08cd76ff43341bea971fb88f4e1bfd8
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08357679B2

반응 노트

불러오는 중…