Methanol → HCID 69418093, Verbindung

HRID 1375087Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1375087
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([CH2:14][C:15]([OH:17])=[O:16])[CH2:13][CH2:12][O:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[CH3:18]O>S(=O)(=O)(O)O>[CH3:18][O:16][C:15](=[O:17])[CH2:14][C:8]1([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[CH2:9][CH2:10][O:11][CH2:12][CH2:13]1

Komponenten

4

Edukt 2

HCID 887MethanolHCID 210779472-(4-(4-Chlorophenyl)tetrahydro-2H-pyran-4-yl)acetic acid

Produkt 1

HCID 69418093HCID 69418093, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidKatalysator

Versuchsvorschrift

A stirred solution of (4-{4-chloro-phenyl}-tetrahydro-pyran-4-yl)-acetic acid [3.3 g, Reference Example 21(a)] in anhydrous methanol (125 mL), under argon, was treated with concentrated sulfuric acid (8 drops). This mixture was stirred at reflux temperature for 5.5 hours then evaporated. The residue was treated with ethyl acetate (35 mL) and the resulting solution was washed three times with water (10 mL), then dried over magnesium sulfate and then evaporated to give the title compound (3.12 g) as a pale amber oil. LC-MS: RT=3.43 minutes, MS(ES+): 269 and 271(M+H)+.

Aufarbeitung

  1. temperatureat reflux temperature for 5.5 hours
  2. customthen evaporated
  3. additionThe residue was treated with ethyl acetate (35 mL)
  4. washthe resulting solution was washed three times with water (10 mL)
  5. dry with materialdried over magnesium sulfate
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-006855bb233c4a5bbfac880e371c0697
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07166616B2

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