Pyridine → 2-benzyloxyacetophenone O-methyloxime

HRID 484561Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 484561
N1C=CC=CC=1.[CH2:7]([O:14][CH2:15][C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.Cl.[CH3:25][O:26][NH2:27]>O>[CH3:25][O:26][N:27]=[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:15][O:14][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 112531252-(Benzyloxy)-1-phenylethan-1-one

Produkt 1

HCID 541941012-benzyloxyacetophenone O-methyloximeAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To 50 ml of pyridine were added 0.0434 mole (9.77 g) of 2-benzyloxyacetophenone prepared in the first and second paragraphs in Referential Example 1 (Table 1, No. 1) and 4.35 g (0.0521 mole) of O-methylhydroxylamine hydrochloride. The mixture was stirred at room temperature for 2 hours and then at 100° C. for 1 hour. The reaction liquid was cooled down to room temperature, 300 ml of water was added thereto, and the oil layer was separated off. The aqueous layer was extracted with chloroform and the extract was combined with said oil layer, washed with water, dried and distilled under reduced pressure to obtain 10.77 g of 2-benzyloxyacetophenone O-methyloxime.

Aufarbeitung

  1. customprepared in the first and second paragraphs in Referential Example 1 (Table 1
  2. waitat 100° C. for 1 hour
  3. customThe reaction liquid
  4. temperaturewas cooled down to room temperature
  5. customthe oil layer was separated off
  6. extractionThe aqueous layer was extracted with chloroform
  7. washwashed with water
  8. customdried
  9. distillationdistilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-07d450e9f5d0402c8104376b0cc463d9
Quelldatensatz
uspto-grants-1993_07
Patentnummer
US05231227

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