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Isopropanol → (R)-N-((R)-1-(1-benzylpiperidin-4-yl)-1-cyanopent-4-enyl)-2-methylpropane-2-sulfinamide

HRID 579584
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HRID 579584 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11](/[C:14](=[N:19]\[S@@:20]([C:22]([CH3:25])([CH3:24])[CH3:23])=[O:21])/[CH2:15][CH2:16][CH:17]=[CH2:18])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Al]([C:31]#[N:32])(CC)CC.CC(O)C>C1COCC1>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([C@@:14]([NH:19][S@@:20]([C:22]([CH3:25])([CH3:24])[CH3:23])=[O:21])([C:31]#[N:32])[CH2:15][CH2:16][CH:17]=[CH2:18])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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HCID 3776IsopropanolHCID 16683962(cyano-C)diethylaluminiumHCID 87173115(NZ,R)-N-[1-(1-benzylpiperidin-4-yl)pent-4-enylidene]-2-methylpropane-2-sulfinamide

생성물 1

HCID 66833653(R)-N-((R)-1-(1-benzylpiperidin-4-yl)-1-cyanopent-4-enyl)-2-methylpropane-2-sulfinamide수율 67.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

실험 절차

A solution of (R,Z)—N-(1-(1-benzylpiperidin-4-yl)pent-4-enylidene)-2-methylpropane-2-sulfinamide (2.74 g, 7.6 mmol) in THF (130 mL, 0.06 M) was cooled to −78° C. Separately, a 1 M solution of Et2AlCN (11.4 mmol, 11.4 mL) was dissolved in THF (20 mL) and cooled to −78° C. iPrOH (0.64 mL, 8.26 mmol) was added dropwise and the solution was warmed to RT over 20 min, then added dropwise to the sulfinamide solution. The reaction was allowed to warm gradually to RT and stirred overnight. The reaction was quenched with saturated aqueous ammonium chloride (50 mL) and filtered through Celite. The Celite pad was washed with ethyl acetate (3×) and the combined organics were washed saturated aqueous sodium chloride, dried over MgSO4, and concentrated in vacuo. The residue was chromatographed on silica gel (1-9% methanol in dichloromethane and again with 2-5% methanol in ethyl acetate) to afford the desired product (1.99 g, 67%) along with its undesired diastereoisomer (0.46 g, 15%). Rf 0.26 (10% MeOH/CH2Cl2). 1H NMR (CDCl3, 300 MHz) δ 7.31-7.25 (m, 5H), 5.83-5.78 (m, 1H), 5.13-5.03 (m, 2H), 3.51 (d, J=1.5 Hz, 2H), 3.41 (s, 1H), 3.00 (d, J=11.0 Hz, 2H), 2.34-2.29 (m, 2H), 2.05-1.83 (m, 6H), 1.60-1.44 (m, 3H), 1.25 (s, 9H). ESI MS found for C22H33N3OS m/z [388.4 (M+1)].

후처리

  1. additionwas added dropwise
  2. temperatureto warm gradually to RT
  3. customThe reaction was quenched with saturated aqueous ammonium chloride (50 mL)
  4. filtrationfiltered through Celite
  5. washThe Celite pad was washed with ethyl acetate (3×)
  6. washthe combined organics were washed saturated aqueous sodium chloride
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customThe residue was chromatographed on silica gel (1-9% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-2289ecd1f4ca4bfdb55de078a02abeb0
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040703B2

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