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Lithium hydroxide, monohydrate → HCID 53629692, 화합물

HRID 1990042
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HRID 1990042 반응식
O.[OH-].[Li+].CC([Si](C)(C)[O:9][C:10]1[CH:11]=[C:12]([CH:23]=[C:24]([O:26][C@@H:27]([CH3:37])[CH2:28][O:29][Si:30]([C:33]([CH3:36])([CH3:35])[CH3:34])([CH3:32])[CH3:31])[CH:25]=1)[C:13]([NH:15][C:16]1[CH:21]=[N:20][C:19]([CH3:22])=[CH:18][N:17]=1)=[O:14])(C)C>O.C1COCC1>[CH3:34][C:33]([Si:30]([CH3:31])([CH3:32])[O:29][CH2:28][C@@H:27]([O:26][C:24]1[CH:23]=[C:12]([CH:11]=[C:10]([OH:9])[CH:25]=1)[C:13]([NH:15][C:16]1[CH:21]=[N:20][C:19]([CH3:22])=[CH:18][N:17]=1)=[O:14])[CH3:37])([CH3:35])[CH3:36]
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 536296933-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-5-[((1S)-2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-1-methylethyl)oxy]-N-(5-methylpyrazin-2-yl)benzamide

생성물 1

HCID 53629692HCID 53629692, 화합물수율 0.1%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran
용매

실험 절차

Lithium hydroxide monohydrate (0.38 g, 9.12 mol) in water (20 mL) was added to a solution of 3-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-5-[((1S)-2-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-1-methylethyl)oxy]-N-(5-methylpyrazin-2-yl)benzamide (1.94 g, 3.65 mol) in THF (40 mL) and stirred at RT for 20 hours. The THF was removed in vacuo and the aqueous layer was adjusted to pH7. Ethyl acetate (50 mL) and water (50 mL) were added then the aqueous layer re-extracted into ethyl acetate (50 mL) and the combined organics washed with water (50 mL), brine (50 mL), dried (MgSO4), filtered and reduced in vacuo. The crude material was chromatographed on silica, eluting with 20-50% ethyl acetate in isohexane, to give the desired material as a white solid (0.8 g). 1H NMR δ (CDCl3): 0.04 (s, 3H), 0.08 (s, 3H), 0.87 (s, 9H), 1.30 (d, 3H), 2.56 (s, 3H), 3.65-3.81 (m, 2H), 4.46-4.51 (m, 1H), 5.63 (s, 1H), 6.63 (t, 1H), 6.98 (t, 1H), 7.04 (t, 1H), 8.15 (s, 1H), 8.41 (s, 1H), 9.57 (s, 1H); m/z 418 (M+H)+

후처리

  1. customThe THF was removed in vacuo
  2. additionEthyl acetate (50 mL) and water (50 mL) were added
  3. extractionthe aqueous layer re-extracted into ethyl acetate (50 mL)
  4. washthe combined organics washed with water (50 mL), brine (50 mL)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customThe crude material was chromatographed on silica
  8. washeluting with 20-50% ethyl acetate in isohexane

출처 및 근거

ORD 기록
ord-efbc0b5f4c8946e28eb5514cdd90ffed
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07642263B2

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