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Water → HCID 86618695, 화합물

HRID 2239369
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HRID 2239369 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[S:18][C:12]3[C:13](=[O:17])[NH:14][N:15]=[CH:16][C:11]=3[CH:10]=2)=[CH:5][CH:4]=1.[H-].[Na+].CS(O[CH2:26][C:27]1[N:32]=[C:31]([O:33][CH2:34][C@@H:35]2[CH2:40][CH2:39][CH2:38][CH2:37][N:36]2[C:41]([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42])[CH:30]=[CH:29][CH:28]=1)(=O)=O.O>CN(C=O)C.C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[S:18][C:12]3[C:13](=[O:17])[N:14]([CH2:26][C:27]4[N:32]=[C:31]([O:33][CH2:34][C@@H:35]5[CH2:40][CH2:39][CH2:38][CH2:37][N:36]5[C:41]([O:43][C:44]([CH3:47])([CH3:46])[CH3:45])=[O:42])[CH:30]=[CH:29][CH:28]=4)[N:15]=[CH:16][C:11]=3[CH:10]=2)=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 11507160HCID 11507160, 화합물HCID 86618694HCID 86618694, 화합물

생성물 1

HCID 86618695HCID 86618695, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회
HCID 6344
Dichloromethane
용매

실험 절차

To a solution of 2-(4-methoxyphenyl)thieno[2,3-d]pyridazin-7(6H)-one (455 mg, 1.76 mmol) in DMF (5 ml), was added NaH 60% (110 mg, 2.52 mmol) in small portions. The mixture was stirred at rt. for 10 min before addition of tert-butyl (2S)-2-{[(6-{[(methylsulfonyl)oxy]methyl}pyridin-2-yl)oxy]methyl}piperidine-1-carboxylate (672 mg, 1.68 mmol) dissolved in DMF (3 ml). The reaction was stirred at rt. for 16 h, water (150 ml) and DCM (150 ml) added and the phases separated. The aqueous phase was extracted with DCM (150 ml). The combined organic phases were dried through a phase separator and evaporated in vacuo. Purification by silica gel flash chromatography using a 40+M Biotage column with a gradient of 30-100% EtOAc in heptane yielded the title compound as a light yellow solid. Yield: 354 mg (36%). 1H NMR (400 MHz, CDCl3) δ 8.17 (s, 1H), 7.61 (m, 2H), 7.46 (t, 1H, J=7.8 Hz), 7.34 (s, 1H), 6.96 (m, 2H), 6.71 (d, 1H, J=7.3 Hz), 6.55 (d, 1H, J=8.2 Hz), 5.47 (s, 2H), 4.50 (m, 1H), 4.30 (m, 2H), 3.94 (d, 1H, J=10.7 Hz), 3.85 (s, 3H), 2.74 (t, 1H, J=12.2 Hz), 1.67-1.20 (m, 15H). MS (ESI+) 563.30 (M+1H+)

후처리

  1. stirringThe reaction was stirred at rt
  2. customthe phases separated
  3. extractionThe aqueous phase was extracted with DCM (150 ml)
  4. customThe combined organic phases were dried through a phase separator
  5. customevaporated in vacuo
  6. customPurification by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-8ab31b070f434f628b2406b9e1d94c37
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07723331B2

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