Methanol → 4,4-Dimethoxytetrahydro-2H-pyran-3-ol

HRID 1436747

Reaktionsgleichung

Reaktionsgleichung von HRID 1436747
[CH3:1][O:2][C:3]1[CH2:4][CH2:5][O:6][CH2:7][CH:8]=1.ClC1C=CC=C([C:16](OO)=[O:17])C=1.C[OH:21]>>[CH3:1][O:2][C:3]1([O:17][CH3:16])[CH2:4][CH2:5][O:6][CH2:7][CH:8]1[OH:21]

Komponenten

4

Versuchsvorschrift

To a solution of 4-methoxy-3,6-dihydro-2H-pyran (5.00 g, 43.8 mmol) in methanol (100 mL) at 0° C. was dropwise added a solution of m-chloroperbenzoic acid (15.1 g, 87.6 mmol) in methanol (15 mL). After being stirred for 5 h, methanol was removed in vacuo and the white residue was dissolved in methylene chloride (300 mL). To the solution was added K2CO3. The resulting solution was stirred for 1 h and filtered through celite. The filtrate was evaporated in vacuo to provide the desired product which was used directly for the next reaction without purification.

Aufarbeitung

  1. custommethanol was removed in vacuo
  2. dissolutionthe white residue was dissolved in methylene chloride (300 mL)
  3. additionTo the solution was added K2CO3
  4. stirringThe resulting solution was stirred for 1 h
  5. filtrationfiltered through celite
  6. customThe filtrate was evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-a522f38e36d0493d8fee958960b0b03b
Quelldatensatz
uspto-grants-2009_11
Patentnummer
US07618970B2

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