Hydrochloric Acid → 6-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-carboxamide

HRID 510822ノート

反応式

HRID 510822 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([Cl:20])[C:7]([CH3:19])=[C:8]([C:17]#[N:18])[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1)(=[O:3])[CH3:2].[OH-:21].[K+].Cl>C(O)C>[C:1]([C:4]1[CH:5]=[C:6]([Cl:20])[C:7]([CH3:19])=[C:8]([C:17]([NH2:18])=[O:21])[C:9]=1[C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([F:16])[CH:11]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 583684696-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-carbonitrile

生成物 1

HCID 866667626-Acetyl-4-chloro-3'-fluoro-3-methylbiphenyl-2-carboxamide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 6-acetyl-4-chloro-3′-fluoro-3-methylbiphenyl-2-carbonitrile (0.87 g, 3.0 mmol) and potassium hydroxide (0.34 g, 6.1 mmol) in ethanol (4 mL) was refluxed for 2 hours. The mixture was cooled, acidified with 1 N HCl, and extracted with ethyl acetate. The combined organic layers were washed with brine, dried over magnesium sulfate, and evaporated to dryness under reduced pressure to yield the crude product. LCMS calculated for C16H14ClFNO2 (M+H)+: m/z=306.1. found: 306.0.

後処理

  1. temperaturewas refluxed for 2 hours
  2. temperatureThe mixture was cooled
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-20d449cd2b9846cbaa0a96ccd8340865
出典データセット
uspto-grants-2015_08
特許番号
US09096600B2

反応ノート

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