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Diisopropylethylamine → HCID 24852186, 화합물

HRID 2245373
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HRID 2245373 반응식
[I-].C[N+]1C=C[N:5]([C:8](=[O:30])/[N:9]=[C:10]2\[S:11][C:12]([CH3:29])=[CH:13][N:14]\2[C:15]2[CH:28]=[CH:27][C:18]3[O:19][C:20]([F:26])([F:25])[C:21]([F:24])([F:23])[O:22][C:17]=3[CH:16]=2)[CH:4]=1.[F:31][C:32]1[CH:33]=[CH:34][C:35]([O:41][C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)=[C:36](CNC)[CH:37]=1.[CH3:48]CN(C(C)C)C(C)C>C(#N)C.C(Cl)Cl>[F:31][C:32]1[CH:33]=[CH:34][C:35]([O:41][C:42]2[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=2)=[C:36]([CH:37]=1)[CH2:4][N:5]([CH3:48])[C:8](/[N:9]=[C:10]1\[S:11][C:12]([CH3:29])=[CH:13][N:14]\1[C:15]1[CH:28]=[CH:27][C:18]2[O:19][C:20]([F:26])([F:25])[C:21]([F:23])([F:24])[O:22][C:17]=2[CH:16]=1)=[O:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 81531DiisopropylethylamineHCID 242088151-(5-fluoro-2-phenoxyphenyl)-N-methylmethanamineHCID 87462668HCID 87462668, 화합물

생성물 1

HCID 24852186HCID 24852186, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매HCID 6344Dichloromethane
용매

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온도
60 °C

실험 절차

To a solution of Example 81A (0.1 g, 0.18 mmol) and 1-(5-fluoro-2-phenoxyphenyl)-N-methylmethanamine (0.20 mmol) in anhydrous acetonitrile (3 mL) was added Hunig's base (0.025 g), and the solution was heated at 60° C. for 3 hours. After cooling to room temperature, the reaction mixture was diluted with 50 mL of CH2Cl2 and washed with water and brine, dried over sodium sulfate, and concentrated under reduced pressure. The crude residue was choromatographed over silica using CH2Cl2 to give the titled compound. 1H NMR (CD3OD) δ ppm 2.25 (3H), 2.90 (3H), 4.60 (2H), 6.90-7.60 (12H); MS (ESI) 578 (M+H)+.

후처리

  1. temperatureAfter cooling to room temperature
  2. washwashed with water and brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-759e28dde36d48cb8b482caa8984dd23
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07683084B2

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