Diethyl Ether → 3-Hydroxy-2,2-dimethyl-1-propylthiocyanate

HRID 1590054Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1590054
Br[CH2:2][C:3]([CH3:7])([CH3:6])[CH2:4][OH:5].[S-:8][C:9]#[N:10].[K+].CN(C)C=O.C(OCC)C>O>[OH:5][CH2:4][C:3]([CH3:7])([CH3:6])[CH2:2][S:8][C:9]#[N:10]

Komponenten

6

Edukt 4

HCID 3283Diethyl EtherHCID 6228DimethylformamideHCID 1425013-Bromo-2,2-dimethyl-1-propanolHCID 516872Potassium thiocyanate

Produkt 1

HCID 104644533-Hydroxy-2,2-dimethyl-1-propylthiocyanateAusbeute 85,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 16.7 g of 3-bromo-2,2-dimethyl-1-propanol, 14.6 g of potassium thiocyanate and 60 ml of dimethylformamide was stirred for 4 hours at 130°- 140° C. The reaction solution was cooled to room temperature (hereinafter means "5°-20° C."), to which a mixture of 200 ml of diethyl ether and 200 ml of water was added. The ethereal layer was collected. The aqueous layer was extracted with 150 ml of diethyl ether. The combined ethereal layers were washed with a saturated saline, dried over anhydrous magnesium sulfate and distilled to remove the solvent. The residue was distilled under reduced pressure to obtain 12.4 g of 3-hydroxy-2,2-dimethyl-1-propylthiocyanate.

Aufarbeitung

  1. custom"5°-20° C."
  2. additionwas added
  3. customThe ethereal layer was collected
  4. extractionThe aqueous layer was extracted with 150 ml of diethyl ether
  5. washThe combined ethereal layers were washed with a saturated saline
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationdistilled
  8. customto remove the solvent
  9. distillationThe residue was distilled under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-82ce47535036476ebadf104d6d9a371b
Quelldatensatz
uspto-grants-1993_04
Patentnummer
US05202324

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