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Water → 1-[2-Bromo-5,6-dichloro-1-(4-hydroxy-5-hydroxymethyl-tetrahydro-furan-2-yl)-1H-indol-3-yl]-ethanone

HRID 1863857
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HRID 1863857 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[N:7]([C@@H:12]1[O:26][C@H:25]([CH2:27][O:28]C(C3C=CC(C)=CC=3)=O)[C@@H:14]([O:15]C(C3C=CC(C)=CC=3)=O)[CH2:13]1)[C:6]([Br:38])=[C:5]2[C:39](=[O:41])[CH3:40].C[O-].[Na+].O>CO>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[Cl:11])[N:7]([C@@H:12]1[O:26][C@H:25]([CH2:27][OH:28])[C@@H:14]([OH:15])[CH2:13]1)[C:6]([Br:38])=[C:5]2[C:39](=[O:41])[CH3:40]
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참가 물질

5

반응물 3

HCID 962WaterHCID 10942334Sodium MethoxideHCID 67099812HCID 67099812, 화합물

생성물 1

HCID 52726201-[2-Bromo-5,6-dichloro-1-(4-hydroxy-5-hydroxymethyl-tetrahydro-furan-2-yl)-1H-indol-3-yl]-ethanone수율 68%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

5,6-Dichloro-2-bromo-3-acetyl-1-[3,5-di-O-(p-toluoyl)-2-deoxy-β-D-ribofuranosyl]indole (4.142, 1.24 g, 1.7 mmol) was suspended in absolute MeOH (75 mL) to which was added sodium methoxide (250 mg, 4.6 mmol). The suspension was stirred at room temperature for 2 h, after which time the solution first clarified and then a precipitate formed. Water (100 mL) was added, and the suspension was evaporated until no more MeOH remained. The remaining solids were filtered and recrystallized twice from MeOH/H2O to yield 475 mg (68%) of 4.143 as a white crystalline solid: mp slow dec. >235° C.; Rf0.5 (10% MeOH/CHCl3); 1H-NMR (500 MHz, DMSO-d6): δ 8.57 (s, 1H), 8.37 (s, 1H), 6.56 (dd, 1H), 5.46 (s, 1H, D2O exch.), 5.31 (s, 1H, D2O exch.), 4.48 (d, 1H), 3.92 (d, 1H), 3.76 (s, 2H), 2.65 (s, 3H), 2.48 (m, 1H), 2.13 (ddd, 1H). 13C-NMR (125 MHz, DMSO-d6): δ 192.59, 133.20, 126.74, 125.89, 125.77, 121.91, 121.80, 115.94, 115.32, 87.59, 87.30, 69.84, 60.66, 39.23 (under DMSO), 30.95. HRMS (EI) m/z calcd. for C15H14BrCl2NO4 420.9483, found 420.9493. Anal calcd for C15H14BrCl2NO4: C, 42.58; H, 3.34; N, 3.31. Found: C, 42.77; H, 3.25; N, 3.22.

후처리

  1. customa precipitate formed
  2. customthe suspension was evaporated until no more MeOH
  3. filtrationThe remaining solids were filtered
  4. customrecrystallized twice from MeOH/H2O

출처 및 근거

ORD 기록
ord-816e2b038b814ef3a7cd796c8c6d99e7
출처 데이터셋
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07625871B2

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