Hydrochloric Acid → HCID 57780986, Verbindung

HRID 1011227Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1011227
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:23][CH3:24])[C:11]=1[N:12]1[CH2:17][CH2:16][CH:15]([C:18]([O:20]CC)=[O:19])[CH2:14][CH2:13]1)[N:8]([CH2:25][CH2:26][F:27])[CH:7]=[C:6]([C:28]([NH:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([O:38][C:39]([F:42])([F:41])[F:40])=[CH:34][C:33]=1[CH3:43])=[O:29])[C:5]2=[O:44].[OH-].[Li+].Cl>O1CCOCC1.C(OCC)(=O)C.O>[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([O:23][CH3:24])[C:11]=1[N:12]1[CH2:13][CH2:14][CH:15]([C:18]([OH:20])=[O:19])[CH2:16][CH2:17]1)[N:8]([CH2:25][CH2:26][F:27])[CH:7]=[C:6]([C:28]([NH:30][CH2:31][C:32]1[CH:37]=[CH:36][C:35]([O:38][C:39]([F:42])([F:40])[F:41])=[CH:34][C:33]=1[CH3:43])=[O:29])[C:5]2=[O:44]

Komponenten

7

Edukt 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 57781005HCID 57781005, Verbindung

Produkt 1

HCID 57780986HCID 57780986, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

60 mg (0.096 mmol) of the compound of Example 4 are dissolved in 2.35 ml of dioxane, 480 μl (5 eq.) of a 1M solution of lithium hydroxide are added, and the mixture is stirred at RT until the reaction is complete (4 h). The reaction mixture is acidified with 1N hydrochloric acid and diluted with ethyl acetate and water. Following phase separation, the organic phase is washed once again with water and then with a saturated sodium chloride solution, dried over magnesium sulfate and freed from solvents on a rotary evaporator. The residue is dried under high vacuum. 54 mg (94% of theory) of the title compound are obtained.

Aufarbeitung

  1. custom(4 h)
  2. customFollowing phase separation
  3. washthe organic phase is washed once again with water
  4. dry with materialwith a saturated sodium chloride solution, dried over magnesium sulfate
  5. customfreed from solvents on a rotary evaporator
  6. customThe residue is dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-915291128ce9417094a5cafe476c59c8
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07977349B2

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