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Imidazole → HCID 22005186, 화합물

HRID 324874
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HRID 324874 반응식
[CH:1]([C:4]1[C:9]([CH2:10][OH:11])=[C:8]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[C:7]([CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[C:6]([CH:24]([CH3:26])[CH3:25])[N:5]=1)([CH3:3])[CH3:2].N1C=CN=C1.[Si:32](Cl)([C:35]([CH3:38])([CH3:37])[CH3:36])([CH3:34])[CH3:33]>C(Cl)Cl>[CH:1]([C:4]1[C:9]([CH2:10][O:11][Si:32]([C:35]([CH3:38])([CH3:37])[CH3:36])([CH3:34])[CH3:33])=[C:8]([C:12]2[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=2)[C:7]([CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[C:6]([CH:24]([CH3:25])[CH3:26])[N:5]=1)([CH3:3])[CH3:2]
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참가 물질

5

반응물 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 220049552,6-Diisopropyl-3-hydroxymethyl-4-(4-fluorophenyl)-5-pentylpyridine

생성물 1

HCID 22005186HCID 22005186, 화합물수율 79%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
25 °C

실험 절차

To a solution of 2,6-diisopropyl-3-hydroxymethyl-4-(4-fluorophenyl)-5-pentylpyridine (3.14 g, 8.78 mmol) (Example 1, Step H) in methylene chloride (45 mL) were added imidazole (0.9 g, 13.17 mmol, 1.5 eq) and t-butyl-dimethylsilyl chloride (2.0 g, 13.17 mmol, 1.5 eq). A white precipitate began to form immediately. The mixture was stirred for 14 h at 25° C. and was then diluted with methylene chloride (100 mL) and washed sequentially with 10% hydrochloric add (20 mL), saturated aqueous sodium bicarbonate (20 mL), and brine (20 mL). The organic layer was concentrated under reduced pressure and the resultant residue was recrystallized from methanol to provide the product (3.27 g, 79%) as a white fluffy crystalline solid. 1H NMR (300 MHz, CDCl3): δ −0.10 (s, 6 H), 0.79 (t, J=6.9 Hz, 3 H), 0.83 (s, 9 H), 1.07-1.20 (m, 4 H), 1.29-1.32 (m, 14 H), 2.23-2.30 (m, 2 H), 3.21 (sept, J=6.6 Hz, 1 H), 3.35 (sept, J=6.6 Hz, 1 H), 4.24 (s, 2 H), 7.05-7.18 (m, 4 H). Anal. calc. for C29H46NOFSi: C, 73.83; H, 9.83; N, 2.97. Found: C, 73.82; H, 9.95; N, 2.86.

후처리

  1. customto form immediately
  2. washwashed sequentially with 10%
  3. additionhydrochloric add (20 mL), saturated aqueous sodium bicarbonate (20 mL), and brine (20 mL)
  4. concentrationThe organic layer was concentrated under reduced pressure
  5. customthe resultant residue was recrystallized from methanol

출처 및 근거

ORD 기록
ord-f1de5303106547779b95f827f5fee975
출처 데이터셋
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06218431B1

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