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Methyl iodide → 1-cyclopropyl-5,6-difluoro-2-[5-(2-methoxypropan-2-yl)pyridin-3-yl]-1H-benzimidazole

HRID 1048957
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HRID 1048957 반응식
[CH:1]1([N:4]2[C:8]3[CH:9]=[C:10]([F:14])[C:11]([F:13])=[CH:12][C:7]=3[N:6]=[C:5]2[C:15]2[CH:16]=[C:17]([C:21]([OH:24])([CH3:23])[CH3:22])[CH:18]=[N:19][CH:20]=2)[CH2:3][CH2:2]1.[H-].[Na+].I[CH3:28]>O1CCCC1.C(OCC)(=O)C>[CH:1]1([N:4]2[C:8]3[CH:9]=[C:10]([F:14])[C:11]([F:13])=[CH:12][C:7]=3[N:6]=[C:5]2[C:15]2[CH:20]=[N:19][CH:18]=[C:17]([C:21]([O:24][CH3:28])([CH3:22])[CH3:23])[CH:16]=2)[CH2:3][CH2:2]1
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참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 566455682-[5-(1-Cyclopropyl-5,6-difluoro-1H-benzimidazol-2-yl)pyridin-3-yl]propan-2-ol

생성물 1

HCID 666847641-cyclopropyl-5,6-difluoro-2-[5-(2-methoxypropan-2-yl)pyridin-3-yl]-1H-benzimidazole

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a cooled (0° C.) solution of 2-[5-(1-Cyclopropyl-5,6-difluoro-1H-benzimidazol-2-yl)pyridin-3-yl]propan-2-ol (from Example 38 Step E) (0.086 g, 0.26 mmol) in tetrahydrofuran (1.3 mL) was added sodium hydride (60% dispersion in mineral oil, 0.026 g, 0.65 mmol). After 1 hour, iodomethane (0.024 mL, 0.389 mmol) was added. The reaction was then warmed to room temperature and stirred overnight. The reaction mixture was diluted with ethyl acetate, washed with water and brine, dried over magnesium sulfate, filtered and concentrated. Purification by flash chromatography on silica gel (30-60% ethyl acetate in hexanes) provided the title compound: LCMS m/z 344.03 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 9.09 (d, J=1.9 H, 1 H), 8.79 (d, J=2.0 Hz, 1 H), 8.29 (t, J=2.0, 2.0 Hz, 1 H), 7.58 (dd, J=10.3, 7.3 Hz, 1 H), 7.40 (dd, J=9.7, 7.1 Hz, 1 H), 3.59-3.57 (m, 1 H), 3.16 (s, 3 H), 1.63 (s, 3 H), 1.60 (s, 3 H), 1.20-1.17 (m, 2 H), 0.79-0.76 (m, 2 H).

후처리

  1. washwashed with water and brine
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customPurification by flash chromatography on silica gel (30-60% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-aeaec93be35f41a6b4795fe06c1338ec
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382226B2

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