Trifluoroacetic acid → HCID 12943342、化合物

HRID 659132

反応式

HRID 659132 の反応式
[C:1]1([CH:7]([NH:11]C(=O)OC(C)(C)C)[CH2:8][C:9]#[CH:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>ClCCl>[C:1]1([CH:7]([NH2:11])[CH2:8][C:9]#[CH:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 57429813Tert-butyl (1-phenylbut-3-yn-1-yl)carbamate2 回

生成物 1

HCID 12943342HCID 12943342、化合物収率 93%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1.03 g of tert-butyl 1-phenylbut-3-ynylcarbamate (Formula 16) in 15 mL of dichloromethane was added 3 mL of trifluoroacetic acid. The mixture was stirred at room temperature for 1 hour. Then, dichloromethane was removed. The residue was diluted with water and extracted with ethyl acetate. Combined ethyl acetate was washed with brine, dried over sodium sulfate and concentrated. Column chromatography (60% ethyl acetate/hexane) gave 564 mg (93%) of 1-phenylbut-3-yn-1-amine (Formula 17) as a clear oil. 1H NMR (300 MHz, CDCl3) δ 2.04-2.05 (m, 1H), 2.43-2.63 (m, 2H), 4.14-4.19 (m, 1H), 7.24-7.40 (m, 5H).

後処理

  1. customThen, dichloromethane was removed
  2. additionThe residue was diluted with water
  3. extractionextracted with ethyl acetate
  4. washCombined ethyl acetate was washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-0e2bc74570eb498687da572516211016
出典データセット
uspto-grants-2011_12
特許番号
US08080570B2

関連ノート

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