Water → 2-(Hydroxymethyl)-7-methoxy-9H-xanthen-9-OL

HRID 436000

Reaktionsgleichung

Reaktionsgleichung von HRID 436000
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][C:9]1[CH:22]=[C:21]2[C:12]([O:13][C:14]3[CH:15]=[CH:16][C:17]([C:24](OCC)=[O:25])=[CH:18][C:19]=3[C:20]2=[O:23])=[CH:11][CH:10]=1.O.[O-]S([O-])(=O)=O.[Mg+2]>C1COCC1>[OH:23][CH:20]1[C:19]2[CH:18]=[C:17]([CH2:24][OH:25])[CH:16]=[CH:15][C:14]=2[O:13][C:12]2[C:21]1=[CH:22][C:9]([O:8][CH3:7])=[CH:10][CH:11]=2

Komponenten

6

Edukt 4

HCID 962WaterHCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 21455094Ethyl 7-methoxy-9-oxo-9H-xanthene-2-carboxylate

Produkt 1

HCID 214550952-(Hydroxymethyl)-7-methoxy-9H-xanthen-9-OLAusbeute 84 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Lithium aluminum hydride (500 mg) was added to a stirred solution of ethyl 7-methoxy-9-oxoxanthene-2-carboxylate (1g) in THF (100 ml). The reaction mixture was stirred at room temperature under nitrogen for 5 hours. Water and MgSO4 were added. The inorganic solids were filtered off and washed with ethyl acetate. The filtrate and washings were combined and evaporated to give the crude product. Recrystallization from ethyl acetate gave white crystals (0.82 g, 84%), mp. 142°-143°.

Aufarbeitung

  1. filtrationThe inorganic solids were filtered off
  2. washwashed with ethyl acetate
  3. customevaporated
  4. customto give the crude product
  5. customRecrystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-67a38b1b31974630bd45356f0540d6db
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04007205

Verknüpfte Notizen

Wird geladen…