HCID 15027234、化合物 → N-(2-Carbomethoxy-6-chlorophenyl)acetamide

HRID 974414ノート

反応式

HRID 974414 の反応式
[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]

参加物

3

反応物 1

HCID 15027234HCID 15027234、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0d7360e83951429ba36dbb7e1393ef0c
出典データセット
uspto-grants-1991_11
特許番号
US05068392

反応ノート

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