HCID 67059672、化合物 → HCID 67059665、化合物

HRID 1807772ノート

反応式

HRID 1807772 の反応式
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

参加物

6

反応物 2

HCID 67059672HCID 67059672、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 67059665HCID 67059665、化合物収率 73.8%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d08cd76ff43341bea971fb88f4e1bfd8
出典データセット
uspto-grants-2013_01
特許番号
US08357679B2

反応ノート

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