trans-Ethyl 3-(4-cyano-3-fluorophenyl)-2-propenoate → Ethyl 4-cyano-3-fluorophenylpropanoate

HRID 412192ノート

反応式

HRID 412192 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6](/[CH:9]=[CH:10]/[C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:5][C:4]=1[F:16])#[N:2]>CO.[Pd]>[C:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])=[CH:5][C:4]=1[F:16])#[N:2]

参加物

4

反応物 1

HCID 23021829trans-Ethyl 3-(4-cyano-3-fluorophenyl)-2-propenoate

生成物 1

HCID 18536111Ethyl 4-cyano-3-fluorophenylpropanoate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a solution of the product from Step B (1.3 g, 5.9 mmol) in 30 mL of methanol was added 10% palladium on carbon (130 mg). The solution was stirred at room temperature under an atmosphere of hydrogen for 2 hours, then purged with argon. The mixture was filtered through celite, the filter pad was washed with methanol, and the filtrate was concentrated in vacuo. The crude product was purified on a C18 preparative HPLC column to give the titled product after conversion to the free base.

後処理

  1. custompurged with argon
  2. filtrationThe mixture was filtered through celite
  3. washthe filter pad was washed with methanol
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe crude product was purified on a C18 preparative HPLC column

出典と根拠

ORDレコード
ord-5c5b2f468a4446d6b5f3a3c1ffad90d1
出典データセット
uspto-grants-2003_05
特許番号
US06562823B1

反応ノート

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