Potassium Carbonate → 1,3-Difluoro-5-methyl-2-nitrobenzene

HRID 2061502ノート

反応式

HRID 2061502 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH2:12]C(O)=O)[CH:5]=[C:6]([F:11])[C:7]=1[N+:8]([O-:10])=[O:9].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[F:1][C:2]1[CH:3]=[C:4]([CH3:12])[CH:5]=[C:6]([F:11])[C:7]=1[N+:8]([O-:10])=[O:9]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 179671372-(3,5-Difluoro-4-nitrophenyl)acetic acid

生成物 1

HCID 569244411,3-Difluoro-5-methyl-2-nitrobenzene

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

A mixture of (3,5-difluoro-4-nitrophenyl)acetic acid (41 g), potassium carbonate (24.6 g) and DMF (205 ml) was slowly heated to about 50° C. for 30 minutes. The reaction was then cooled to about 25° C. and quenched into 2M HCl (1025 ml) and hexane (400 ml) and stirred for 10 minutes. The layers were separated and the aqueous layer was extracted with hexane (400 ml). The combined hexane layers were washed with saturated brine (2×200 ml), then dried with anhydrous sodium sulphate and the solution was concentrated to give the title compound as a low melting solid (26 g).

後処理

  1. temperatureThe reaction was then cooled to about 25° C.
  2. customquenched into 2M HCl (1025 ml) and hexane (400 ml)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with hexane (400 ml)
  5. washThe combined hexane layers were washed with saturated brine (2×200 ml)
  6. dry with materialdried with anhydrous sodium sulphate
  7. concentrationthe solution was concentrated

出典と根拠

ORDレコード
ord-683fc03191cf48ceb0bdb79f8df44ec9
出典データセット
uspto-grants-2012_10
特許番号
US08283364B2

反応ノート

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