Triethylamine → HCID 178506375, 화합물

HRID 419741노트

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HRID 419741 반응식
[F:1][C:2]([F:22])([F:21])[O:3][C:4]1[CH:5]=[C:6]([C:10]2[N:11]=[C:12]([CH:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)[NH:13][CH:14]=2)[CH:7]=[CH:8][CH:9]=1.Cl[C:24]1[N:32]=[CH:31][N:30]=[C:29]2[C:25]=1[NH:26][CH:27]=[N:28]2.C(N(CC)CC)C>CC(O)C>[F:22][C:2]([F:1])([F:21])[O:3][C:4]1[CH:5]=[C:6]([C:10]2[N:11]=[C:12]([CH:15]3[CH2:16][CH2:17][N:18]([C:24]4[N:32]=[CH:31][N:30]=[C:29]5[C:25]=4[NH:26][CH:27]=[N:28]5)[CH2:19][CH2:20]3)[NH:13][CH:14]=2)[CH:7]=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 53592776-ChloropurineHCID 178506376HCID 178506376, 화합물

생성물 1

HCID 178506375HCID 178506375, 화합물수율 65%

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
80 °C

실험 절차

Add 4-(4-(3-(trifluoromethoxy)phenyl)-1H-imidazol-2-yl)piperidine (200 mg, 0.642 mmol), 6-chloropurine (105 mg, 0.679 mmol), and triethylamine (95 μL, 0.681 mmol) to 2-propanol (5 mL). Heat the mixture at 80° C. for 3 h. Cool the mixture to room temperature and concentrate in vacuo. Triturate the solid in CH2Cl2 (10 mL). Purify the remaining solid by silica gel chromatography (60 g, eluting with 40% methanol/methylene chloride, 0.500 L) to provide 6-(4-(4-(3-(trifluoromethoxy)phenyl)-1H-imidazol-2-yl)piperidin-1-yl)-7H-purine (179 mg, 65%).

후처리

  1. temperatureCool the mixture to room temperature
  2. concentrationconcentrate in vacuo
  3. customTriturate the solid in CH2Cl2 (10 mL)
  4. customPurify the remaining solid
  5. washby silica gel chromatography (60 g, eluting with 40% methanol/methylene chloride, 0.500 L)

출처 및 근거

ORD 기록
ord-06ae26d13ac24e6ca8eeb1fb873fa3c6
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08093383B2

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