HCID 17986946、化合物 → 4-(4-Fluorophenyl)butanenitrile

HRID 1376280ノート

反応式

HRID 1376280 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][CH2:10][C:11]([NH2:13])=O)=[CH:4][CH:3]=1>FC(F)(F)C(OC(=O)C(F)(F)F)=O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][CH2:9][CH2:10][C:11]#[N:13])=[CH:6][CH:7]=1

参加物

3

反応物 1

HCID 17986946HCID 17986946、化合物

生成物 1

HCID 198754764-(4-Fluorophenyl)butanenitrile収率 100%

試薬・触媒・溶媒 1

HCID 9845Trifluoroacetic anhydride溶媒

実験手順

4(4-Fluorophenyl)-butyramide (Int. A4) (2.63 g) was dissolved in trifluoroacetic anhydride (10 ml) and stirred for 2 h. The solution was concentrated and then dissolved in dichloromethane and washed with 2N sodium hydroxide solution. The organics extracts were isolated, dried (MgSO4) and concentrated to yield the product (2.3 g, 100%) which contained ˜5% starting amide as an impurity. 1H-NMR (CDCl3) δ 1.96 (2H, app q), 2.31 (2H, t), 2.75 (2H, t), 6.98 (2H, m), 7.14 (2H, m). MS (APCI+)M+1=164, C10H10FN requires 163.

後処理

  1. concentrationThe solution was concentrated
  2. dissolutiondissolved in dichloromethane
  3. washwashed with 2N sodium hydroxide solution
  4. customThe organics extracts were isolated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0b5fbeb9068747b3ad677d2c61cdfdea
出典データセット
uspto-grants-2007_01
特許番号
US07169924B2

反応ノート

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