Hydrogen Peroxide → HCID 178429771, Verbindung

HRID 1419810Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1419810
[CH3:1][C:2]1([CH:5]2[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]2)[CH2:4][CH2:3]1.CCC(C)[BH-](C(C)CC)C(C)CC.[Li+].[OH-].[Na+].OO>C1COCC1.C(O)C.O>[CH3:1][C:2]1([C@@H:5]2[CH2:10][CH2:9][C@H:8]([OH:11])[CH2:7][CH2:6]2)[CH2:3][CH2:4]1

Komponenten

8

Versuchsvorschrift

A solution of 4.0 g (26.3 mmol) of 4-(1-methylcyclopropyl)cyclohexanone in 30 ml of THF was added dropwise at -78° C. to 5.5 g (29.0 mmol) of L-Selectride (1M in THF) and the mixture was subsequently stirred for 3 hours. It was then heated to room temperature, and 4 ml of H2O, 15 ml of ethanol, 11 ml of 6N NaOH and 13 ml of 35% strength H2O2 solution were added in succession to the reaction solution. This solution was left to stand overnight and then subjected to aqueous workup. Extraction was carried out with methylene chloride, and the extract was dried and concentrated. 3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.

Aufarbeitung

  1. waitThis solution was left
  2. waitto stand overnight
  3. extractionExtraction
  4. customthe extract was dried
  5. concentrationconcentrated
  6. custom3.4 g (86% of theory) were obtained of a colorless crystal powder, m.p.: 56° to 57° C.

Quellen und Nachweise

ORD-Eintrag
ord-52ab13d1969b4553b3185ba39d940fd3
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05889012

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