HCID 15027234, 화합물 → N-(2-Carbomethoxy-6-chlorophenyl)acetamide

HRID 974414노트

반응식

HRID 974414 반응식
[C:1]([C:5]1[CH:10]=[C:9](Br)[CH:8]=[C:7]([Cl:12])[C:6]=1[NH:13][C:14](=[O:16])[CH3:15])([O:3][CH3:4])=[O:2]>C(O)C>[C:1]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([Cl:12])[C:6]=1[NH:13][C:14](=[O:16])[CH3:15])([O:3][CH3:4])=[O:2]

참가 물질

3

반응물 1

HCID 15027234HCID 15027234, 화합물

생성물 1

HCID 15027235N-(2-Carbomethoxy-6-chlorophenyl)acetamide수율 78.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In a hydrogenation apparatus was placed 3.1 g of N-(2-carbomethoxy-4-bromo-6-chlorophenyl)acetamide and 100 mL of ethanol. The apparatus was purged with nitrogen and 0.1 g of 10 percent palladium on charcoal was added. The mixture was agitated under a hydrogen atmosphere at 40 psig for 2 hr at ambient temperature. The mixture was filtered to remove the catalyst, and the solvent was removed from the filtrate under reduced pressure. The product was purified by elution from a silica gel column using a gradient of 9:1 to 1:1 methylene chloride : ethyl acetate as the eluent to give 1.8 g of white solid (m.p. 135°-136° C.). 1H NMR (acetoned d6 +CDCl3) δ7.92 (d with fine coupling, 8.0 Hz, lH), 7.74 (d with fine coupling, 8.0 Hz, 1H), 7.46 (t, 8.0 HZ, 1H), 3.98 (s, 3H, OCH3), 2.55 (s, 3H, COCH3).

후처리

  1. customThe apparatus was purged with nitrogen and 0.1 g of 10 percent palladium on charcoal
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. customto remove the catalyst
  5. customthe solvent was removed from the filtrate under reduced pressure
  6. customThe product was purified by elution from a silica gel column

출처 및 근거

ORD 기록
ord-0d7360e83951429ba36dbb7e1393ef0c
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05068392

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