Trifluoroacetic acid → HCID 12943342, 화합물

HRID 659132

반응식

HRID 659132 반응식
[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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 57429813Tert-butyl (1-phenylbut-3-yn-1-yl)carbamate2회

생성물 1

HCID 12943342HCID 12943342, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0e2bc74570eb498687da572516211016
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08080570B2

연결된 노트

불러오는 중…