Water → HCID 59634057, Verbindung

HRID 1615059Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1615059
[OH:1][CH2:2][C:3]1([CH2:15][OH:16])[CH2:8][O:7][CH:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[O:5][CH2:4]1.[H-].[Na+].CS(O[CH2:24][C:25]1[CH:30]=[CH:29][N:28]=[C:27]([C:31]([N:33]2[CH2:36][CH:35]([C:37]3[CH:42]=[CH:41][C:40]([O:43][CH2:44][C:45]4[CH:50]=[CH:49][C:48]([CH:51]5[CH2:53][CH2:52]5)=[CH:47][CH:46]=4)=[C:39]([O:54][CH3:55])[CH:38]=3)[CH2:34]2)=[O:32])[CH:26]=1)(=O)=O.O>CN(C=O)C>[CH:51]1([C:48]2[CH:49]=[CH:50][C:45]([CH2:44][O:43][C:40]3[CH:41]=[CH:42][C:37]([CH:35]4[CH2:34][N:33]([C:31]([C:27]5[CH:26]=[C:25]([CH2:24][O:16][CH2:15][C:3]6([CH2:2][OH:1])[CH2:4][O:5][CH:6]([C:9]7[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=7)[O:7][CH2:8]6)[CH:30]=[CH:29][N:28]=5)=[O:32])[CH2:36]4)=[CH:38][C:39]=3[O:54][CH3:55])=[CH:46][CH:47]=2)[CH2:53][CH2:52]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 17042Mono-o-benzylidinepentaerythritolHCID 24758Sodium hydrideHCID 59634043HCID 59634043, Verbindung

Produkt 1

HCID 59634057HCID 59634057, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of (5-hydroxymethyl-2-phenyl-[1,3]dioxan-5-yl)methanol (0.66 g) in DMF (10 mL) was added NaH (0.12 g). The mixture was stirred at RT for 1 hr. To the mixture was added 2-{3-[4-(4-cyclopropylbenzyloxy)-3-methoxyphenyl]azetidine-1-carbonyl}pyridin-4-ylmethyl methanesulfonate (0.7 g) prepared in Example 1 (7). The reaction mixture was stirred at RT for 1 hr. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water, and then dried over MgSO4. The solvent was removed under reduced pressure to give the crude title compound.

Aufarbeitung

  1. stirringThe reaction mixture was stirred at RT for 1 hr
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with water
  4. dry with materialdried over MgSO4
  5. customThe solvent was removed under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-105fbc1a745c44b09dee676c9fe90d76
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08765739B2

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