Sodium hydride → Methyl 4-(5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthyloxy)benzoate

HRID 1275610

Reaktionsgleichung

Reaktionsgleichung von HRID 1275610
[CH3:1][C:2]1([CH3:15])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([OH:14])[CH:5]=[CH:4][C:3]1=2.[H-].[Na+].I[C:19]1[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=1>[Cu](Br)Br.N1C=CC=CC=1>[CH3:1][C:2]1([CH3:15])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([O:14][C:19]3[CH:28]=[CH:27][C:22]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:20]=3)[CH:5]=[CH:4][C:3]1=2

Komponenten

6

Versuchsvorschrift

5.3 g (15 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl-2-naphthol and 70 ml of pyridine were introduced into a three-necked flask under a nitrogen stream, and 430 mg (15 mmol) of sodium hydride (80% in oil) were added in small amounts. The mixture was stirred for 30 minutes, 3.9 g (15 mmol) of methyl 4-iodobenzoate and 4.6 g (22.5 mmol) of a copper bromide and dimethyl sulfide complex were added successively and the resulting mixture was heated at reflux for 16 hours. The reaction medium was evaporated to dryness, taken up in water and ethyl ether, the organic phase decanted off, dried over magnesium sulfate and evaporated.

Aufarbeitung

  1. additionwere added in small amounts
  2. temperaturethe resulting mixture was heated
  3. temperatureat reflux for 16 hours
  4. customThe reaction medium was evaporated to dryness
  5. customethyl ether, the organic phase decanted off
  6. dry with materialdried over magnesium sulfate
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-2f3fa2a9de9e4c4081e8da7291a541f3
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06162815

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