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Trimethylsilyl triflate → HCID 53700596, 화합물

HRID 2227218
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HRID 2227218 반응식
[Br:1][C:2]1[C:10]2[N:9]=[C:8]([Cl:11])[NH:7][C:6]=2[CH:5]=[C:4]([Cl:12])[C:3]=1[Cl:13].C/C(/O[Si](C)(C)C)=N\[Si](C)(C)C.C(O[CH:30]1[O:42][C@H:41]([CH3:43])[C@@H:36]([O:37][C:38](=[O:40])[CH3:39])[C@H:31]1[O:32][C:33](=[O:35])[CH3:34])(=O)C.C[Si](OS(C(F)(F)F)(=O)=O)(C)C>C(#N)C.C(OCC)(=O)C>[Br:1][C:2]1[C:10]2[N:9]=[C:8]([Cl:11])[N:7]([C@@H:30]3[O:42][C@H:41]([CH3:43])[C@@H:36]([O:37][C:38](=[O:40])[CH3:39])[C@H:31]3[O:32][C:33](=[O:35])[CH3:34])[C:6]=2[CH:5]=[C:4]([Cl:12])[C:3]=1[Cl:13]
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참가 물질

7

반응물 4

HCID 65367Trimethylsilyl triflateHCID 6913588N,O-bis(trimethylsilyl)acetamideHCID 11196237Tri-O-acetyl-5-deoxy-D-ribofuranoseHCID 18472159HCID 18472159, 화합물

생성물 1

HCID 53700596HCID 53700596, 화합물수율 55.9%

시약·촉매·용매 2

HCID 6342
Acetonitrile
용매
2회
HCID 8857Ethyl Acetate용매

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온도
65 °C

실험 절차

To a suspension of 4-bromo-2,5,6-trichloro-1H-benzimidazole (0.30 g, 1 mmol), in acetonitrile (5 mL) was added N,O-bis(trimethylsilyl)acetamide (0.25 mL, 1 mmol). The resulting mixture was allowed to stir at 65° C. for 15 min., followed by the addition of 1,2,3-tri-O-acetyl-5-deoxyribofuranose (0.31 g, 1.2 mmol) in acetonitrile (5 mL) and trimethylsilyltrifluoromethane sulfonate (0.25 mL, 1.3 mmol). The mixture was allowed to stir at 65° C. for 20 min and was then allowed to cool to RT. The mixture was diluted with ethyl acetate and was washed with a saturated NaHCO3/NaCl solution, dried over MgSO4 and the solvents were removed by rotary evaporation. The product was purified by flash chromatography using chloroform as eluent followed by recrystallization from methanol to provide 0.28 g (55%) of the title compound as white crystals; m.p. 138-141° C.; 1H NMR (DMSO-d6) δ: 8.18 (s, 1H), 6.19 (d, 1H), 5.61 (dd, 1H), 5.25 (dd, 1H), 4.24 (m, 1H), 2.14 (s, 3H), 2.02 (s, 3H), 1.50 (d, 3H).

후처리

  1. stirringto stir at 65° C. for 20 min
  2. temperatureto cool to RT
  3. washwas washed with a saturated NaHCO3/NaCl solution
  4. dry with materialdried over MgSO4
  5. customthe solvents were removed by rotary evaporation
  6. customThe product was purified by flash chromatography
  7. customfollowed by recrystallization from methanol

출처 및 근거

ORD 기록
ord-62129636baaf43248e9cfa8bf5b031cc
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06413938B1

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