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Potassium Iodide → HCID 66758349, 화합물

HRID 917158
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HRID 917158 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1([CH3:14])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.Br[CH2:16][CH2:17][CH:18]=[C:19]1[C:25]2[CH:26]=[CH:27][CH:28]=[N:29][C:24]=2[CH2:23][O:22][C:21]2[CH:30]=[CH:31][C:32]([C:34]([OH:37])([CH3:36])[CH3:35])=[CH:33][C:20]1=2.[I-].[K+]>C(O)(C)C>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1([CH3:14])[CH2:9][CH2:10][N:11]([CH2:16][CH2:17][CH:18]=[C:19]2[C:25]3[CH:26]=[CH:27][CH:28]=[N:29][C:24]=3[CH2:23][O:22][C:21]3[CH:30]=[CH:31][C:32]([C:34]([OH:37])([CH3:36])[CH3:35])=[CH:33][C:20]2=3)[CH2:12][CH2:13]1
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참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 231369824-(2-Chlorophenyl)-4-methylpiperidineHCID 666859992-[5-(3-Bromo-propylidene)-5,1 1-dihydro-10-oxa-1-aza-dibenzo[a,d]cyclohepten-7-yl]-propan-2-ol

생성물 1

HCID 66758349HCID 66758349, 화합물수율 25%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
80 °C

실험 절차

A solution of 4-(2-Chloro-phenyl)-4-methyl-piperidine (0.29 g, 1.38 mmol) in isopropanol (5 mL) was treated with 2-[5-(3-Bromo-propylidene)-5,11-dihydro-10-oxa-1-aza-dibenzo[a,d]cyclohepten-7-yl]-propan-2-ol (0.19 g, 0.50 mmol) and catalytic potassium iodide. The solution was stirred at 80° C. for 12 hr, and evaporated in vacuo. The residue was purified by silica gel chromatography (ethyl acetate→87:10:3 ethyl acetate/methanol/triethylamine) to yield 0.062 g (25%) of the title compound, 1H-NMR (CDCl3) ∂: 1.10 (3H, s), 1.58 (6H, s), 1.78 (2H, m), 1.90 (1H, m), 2.10 (2H, m), 2.40 (8H, m), 5.30 (2H, brs), 6.18 (1H, t), 6.79(1H, m), 6.92 (1H, m), 7.19–7.39 (6H, m), 7.42 (1H, m), 7.55 (1H, m), 8.55 (1H, d).

후처리

  1. customevaporated in vacuo
  2. customThe residue was purified by silica gel chromatography (ethyl acetate→87:10:3 ethyl acetate/methanol/triethylamine)

출처 및 근거

ORD 기록
ord-de73364aca6e4bb987e9ffa9b1444c66
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07271176B2

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