4-Piperidinone, 2,2,6,6-tetramethyl-, monohydrate → (2,2,6,6-Tetramethyl-4-hydroxy-4-piperidinyl)bis(2-cyanoethyl)phosphine oxide

HRID 918234

Reaktionsgleichung

Reaktionsgleichung von HRID 918234
O.[CH3:2][C:3]1([CH3:12])[CH2:8][C:7](=[O:9])[CH2:6][C:5]([CH3:11])([CH3:10])[NH:4]1.[C:13]([CH2:15][CH2:16][PH:17](=[O:22])[CH2:18][CH2:19][C:20]#[N:21])#[N:14]>C(N(CC)CC)C.C(O)(C)C>[CH3:2][C:3]1([CH3:12])[CH2:8][C:7]([P:17](=[O:22])([CH2:18][CH2:19][C:20]#[N:21])[CH2:16][CH2:15][C:13]#[N:14])([OH:9])[CH2:6][C:5]([CH3:11])([CH3:10])[NH:4]1

Komponenten

5

Edukt 2

HCID 223976024-Piperidinone, 2,2,6,6-tetramethyl-, monohydrateHCID 178511210HCID 178511210, Verbindung

Produkt 1

HCID 21521477(2,2,6,6-Tetramethyl-4-hydroxy-4-piperidinyl)bis(2-cyanoethyl)phosphine oxideAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8471TriethylamineKatalysatorHCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

To 100 milliliters of isopropanol was added 8.65 grams (0.05 mole) of 2,2,6,6-tetramethyl-4-piperidone hydrate; 7.81 grams (0.05 mole) of bis(2-cyanoethyl)phosphine oxide; and 1 gram of triethylamine as catalyst. The reaction mixture was refluxed four hours, cooled in an ice bath, and the crystalline product filtered off. After recrystallization, there was obtained 10.0 grams of white crystalline product of 128°-130°C. melting point, representing a 65% yield.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed four hours
  2. temperaturecooled in an ice bath
  3. filtrationthe crystalline product filtered off
  4. customAfter recrystallization

Quellen und Nachweise

ORD-Eintrag
ord-a7a8c00de87c44faa87768b4ab2ec999
Quelldatensatz
uspto-grants-1976_07
Patentnummer
US03970636

Verknüpfte Notizen

Wird geladen…