Cyclopropylamine → HCID 57687389, 화합물

HRID 559061

반응식

HRID 559061 반응식
F[C:2]1[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=1[C:4]([OH:6])=[O:5].[CH:13]1([NH2:16])[CH2:15][CH2:14]1>N1C=CC=CC=1>[CH:13]1([NH:16][C:2]2[CH:10]=[C:9]([F:11])[CH:8]=[C:7]([F:12])[C:3]=2[C:4]([OH:6])=[O:5])[CH2:15][CH2:14]1

참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 5203732,4,6-Trifluorobenzoic acid

생성물 1

HCID 57687389HCID 57687389, 화합물수율 70.2%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2,4,6-Trifluorobenzoic acid (9.0 g, 34.1 mmol) and cyclopropylamine (14.65 g, 256 mmol) were stirred in pyridine (300 mL) at 120° C. in a sealed tube for 22 h. The solution was concentrated in vacuo. The residue was taken up in water (30 mL) and the solution was acidified to pH 2-3 with 1N HCl. The resulting precipitate was collected by filtration to yield 5.1 g (47%) of clean desired product as a beige solid. 1H NMR (400 MHz, DMSO-d6): δ 8.05 (s, 1H), 6.65 (d, 1H, J=8.0 Hz), 6.42 (t, 1H, J=10.8 Hz), 2.42-2.48 (m, 1H), 0.76-0.83 (m, 2H), 0.45-0.51 (m, 2H). MS (ES) [m+H] calc'd for C10H9F2NO2, 213; found 213.

후처리

  1. concentrationThe solution was concentrated in vacuo
  2. filtrationThe resulting precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-e87a64e4ef554c93bbfde3a7d51289c7
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063066B2

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