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Methyl iodide → HCID 67545272, 화합물

HRID 1619857
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HRID 1619857 반응식
[H-].[Na+].[F:3][CH:4]([F:42])[C:5]1[N:9]([C:10]2[N:15]=[C:14]([N:16]3[CH2:21][CH2:20][O:19][CH2:18][CH2:17]3)[N:13]=[C:12]([C:22]3[CH:27]=[CH:26][C:25]([NH:28][C:29](=[O:35])[O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[CH:24][CH:23]=3)[N:11]=2)[C:8]2[CH:36]=[CH:37][CH:38]=[C:39]([O:40][CH3:41])[C:7]=2[N:6]=1.I[CH3:44]>CN(C=O)C.O>[F:42][CH:4]([F:3])[C:5]1[N:9]([C:10]2[N:15]=[C:14]([N:16]3[CH2:17][CH2:18][O:19][CH2:20][CH2:21]3)[N:13]=[C:12]([C:22]3[CH:23]=[CH:24][C:25]([N:28]([CH3:44])[C:29](=[O:35])[O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[CH:26][CH:27]=3)[N:11]=2)[C:8]2[CH:36]=[CH:37][CH:38]=[C:39]([O:40][CH3:41])[C:7]=2[N:6]=1
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참가 물질

6

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HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 53488103tert-Butyl (4-{4-[2-(difluoromethyl)-4-methoxy-1H-benzimidazol-1-yl]-6-(morpholin-4-yl)-1,3,5-triazin-2-yl}phenyl)carbamate

생성물 1

HCID 67545272HCID 67545272, 화합물수율 85%

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

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온도
0 °C

실험 절차

NaH (95%, 11 mg, 0.435 mmol) was added to a suspension of tert-butyl 4-[4-[2-(difluoromethyl)-4-methoxy-1H-benzimidazol-1-yl]-6-(4-morpholinyl)-1,3,5-triazin-2-yl]phenylcarbamate (Example 74) (120 mg, 0.217 mmol) in DMF (3 mL) at 0° C. After stirring at 0° C. for 15 min, iodomethane (0.020 mL, 0.321 mmol) was added. The reaction mixture was warmed to room temperature, stirred for additional 17 hrs, and then diluted with H2O. The resulting precipitate was collected by filtration and dried to give tert-butyl 4-[4-[2-(difluoromethyl)-4-methoxy-1H-benzimidazol-1-yl]-6-(4-morpholinyl)-1,3,5-triazin-2-yl]phenyl(methyl)carbamate (104 mg, 85%): mp (CH2Cl2/MeOH) 205-208° C.; 1H NMR (CDCl3) δ 8.42 (d, J=8.8 Hz, 2H), 8.09 (dd, J=8.4, 0.6 Hz, 1H), 7.63 (t, JHF=53.5 Hz, 1H), 7.45-7.40 (m, 3H), 6.86 (d, J=7.8 Hz, 1H), 4.13 (m, 2H), 4.07 (s, 3H), 4.00 (m, 2H), 3.86 (m, 4H), 3.35 (s, 3H), 1.50 (s, 9H); Anal. Calcd. for C28H31F2N7O4: C, 59.25; H, 5.5; N, 17.3. Found: C, 59.0; H, 5.3; N, 17.2%.

후처리

  1. temperatureThe reaction mixture was warmed to room temperature
  2. stirringstirred for additional 17 hrs
  3. filtrationThe resulting precipitate was collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-14c6c2904de94ef7b82155ff33ddab54
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772287B2

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