Triethylamine → HCID 178507669, 화합물

HRID 1914841노트

반응식

HRID 1914841 반응식
[NH2:1]/[C:2](/OCC)=[CH:3]\[C:4](=O)[C:5]([F:8])([F:7])[F:6].Cl.[NH2:14][NH2:15].C(N(CC)CC)C>C(O)C>[F:6][C:5]([F:8])([F:7])[C:4]1[CH:3]=[C:2]([NH2:1])[NH:14][N:15]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 115031Hydrazinium chlorideHCID 151117544-Amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one

생성물 1

HCID 178507669HCID 178507669, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of (E)-4-amino-4-ethoxy-1,1,1-trifluorobut-3-en-2-one, (Compound [XXIV]) (7.00 g, 38.2 mmol, 1.0 eq.) in ethanol (150 mL) in a 250 mL round bottom flask was added hydrazine hydrochloride (2.75 g, 40.16 mmol, 1.05 eq.) followed by triethylamine (4.05 g, 40.16 mmol, 1.05 eq.). The reaction mixture was heated to reflux for 16 hours. After cooling and concentration, the residue was purified by silica gel chromatography using CHCl3-MeOH (10%) as the eluant to give Compound [XXV]: LCMS m/e 152 (M+H); 1H NMR (400 MHz, DMSO-d6) δ ppm 5.32 (s, 2H) 5.51 (s, 1H) 12.12 (br. s., 1H).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 16 hours
  3. temperatureAfter cooling
  4. concentrationconcentration
  5. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-565f6522ba874b8aa693394e02a87fdf
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614221B2

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