Pyridine → HCID 11256949, Verbindung

HRID 1602753Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1602753
[C:1](Cl)(=[O:5])[C:2]([CH3:4])=[CH2:3].[CH3:7][Si:8]([Si:11]([Si:19]([CH3:22])([CH3:21])[CH3:20])([Si:15]([CH3:18])([CH3:17])[CH3:16])[CH2:12][CH2:13][OH:14])([CH3:10])[CH3:9].N1C=CC=CC=1>O1CCCC1.C1C2NC3C(=CC=CC=3)SC=2C=CC=1>[C:1]([O:14][CH2:13][CH2:12][Si:11]([Si:19]([CH3:22])([CH3:21])[CH3:20])([Si:15]([CH3:18])([CH3:17])[CH3:16])[Si:8]([CH3:7])([CH3:9])[CH3:10])(=[O:5])[C:2]([CH3:4])=[CH2:3]

Komponenten

6

Edukt 3

HCID 1049PyridineHCID 13528Methacryloyl chlorideHCID 133081222-[1,1,1,3,3,3-Hexamethyl-2-(trimethylsilyl)trisilan-2-yl]ethan-1-ol

Produkt 1

HCID 11256949HCID 11256949, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7108PhenothiazineKatalysatorHCID 8028TetrahydrofuranLösungsmittel2×

Versuchsvorschrift

Methacryloyl chloride (2.50 grams, 0.024 mole) in 25 ml tetrahydro-furan was added dropwise into a solution of 2-tris(trimethylsilyl) silyl ethanol (6.5 grams, 0.022 mole), pyridine (2.0 grams, 0.025 mole) and 25 mg of phenothiazine in 50 ml tetrahydrofuran at room temperature. Stirred at room temperature for two more hours. The solids were filtered off and the solution was washed with 100 ml brine. The solution was then diluted with 100 ml ether and washed with 5% hydrochloric acid, followed by deionzed water, and then with brine. It was dried over anhydrous magnesium sulfate and was concentrated in vacuo. Fractional distillation under reduced pressed gave 5 grams of the product at 105-115° C. at 0.5 mm.

Aufarbeitung

  1. filtrationThe solids were filtered off
  2. washthe solution was washed with 100 ml brine
  3. additionThe solution was then diluted with 100 ml ether
  4. washwashed with 5% hydrochloric acid
  5. dry with materialIt was dried over anhydrous magnesium sulfate
  6. concentrationwas concentrated in vacuo
  7. distillationFractional distillation

Quellen und Nachweise

ORD-Eintrag
ord-66f14550627c402099b9e1e3563baa38
Quelldatensatz
uspto-grants-1999_11
Patentnummer
US05985524

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