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Trifluoroacetic anhydride → HCID 12641099, 화합물

HRID 1504967
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HRID 1504967 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][CH2:12][C:13]([NH2:15])=O)=[CH:6][CH:5]=1)([O-:3])=[O:2].C(OC(C(F)(F)F)=O)(C(F)(F)F)=O>C(Cl)Cl>[N+:1]([C:4]1[CH:5]=[CH:6][C:7]([CH2:10][CH2:11][CH2:12][C:13]#[N:15])=[CH:8][CH:9]=1)([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9845Trifluoroacetic anhydrideHCID 106798654-(4-nitrophenyl)butanamide

생성물 1

HCID 12641099HCID 12641099, 화합물수율 93%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of compound 81 (3.2 g, 22.4 mmol) in DCM (60 mL) was added TEA (10 mL, 77 mmol) at room temperature with stirring. Then to the mixture was added dropwise TFAA (4 mL, 30.8 mmol) at 0° C. The reaction mixture was stirred at room temperature for 4 h. Then the mixture was diluted with DCM, washed by water and brine, dried over Na2SO4 and concentrated to dryness to give compound 82 (2.7 g, 93%) as a yellow oil. 1H NMR (400 MHz, CDCl3) 8.12 (d, 2H, J=8.1 Hz), 7.30 (d, 2H, J=8.1 Hz), 2.85 (t, 2H, J=7.5 Hz), 2.31 (t, 2H, J=7.3 Hz), 1.92-2.05 (m, 2H).

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후처리

  1. stirringThe reaction mixture was stirred at room temperature for 4 h
  2. washwashed by water and brine
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-1d1b7bfb44534f09b33558ae12446aea
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216957B2

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