1-(2,3-Dihydro-1,1,2,3,3-pentamethyl-1H-inden-5-yl)ethan-1-one → HCID 68161383, Verbindung

HRID 1042412

Reaktionsgleichung

Reaktionsgleichung von HRID 1042412
[CH3:1][C:2]1([CH3:17])[C:10]2[C:5](=[CH:6][C:7]([C:11](=O)[CH3:12])=[CH:8][CH:9]=2)[C:4]([CH3:15])([CH3:14])[CH:3]1[CH3:16].[C:18](O)(=O)C.[CH:22]([NH2:24])=[NH:23]>C(O)CCC>[CH3:1][C:2]1([CH3:17])[C:10]2[C:5](=[CH:6][C:7]([C:11]3[CH:12]=[CH:18][N:24]=[CH:22][N:23]=3)=[CH:8][CH:9]=2)[C:4]([CH3:15])([CH3:14])[CH:3]1[CH3:16]

Komponenten

4

Edukt 2

HCID 1073331-(2,3-Dihydro-1,1,2,3,3-pentamethyl-1H-inden-5-yl)ethan-1-oneHCID 160693Formamidine acetate

Produkt 1

HCID 68161383HCID 68161383, VerbindungAusbeute 37,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A 5 L reaction vessel was charged with 1-(1,1,2,3,3-pentamethyl-indan-5-yl)-ethanone (460 g, 2.0 mol) (commercially available at IFF), formamidine acetate (675 g, 6.4 mol), and butanol (1.0 L). The reaction mixture was heated to 120° C. for 10 hours and then cooled to 25° C. The reaction mixture was washed twice with brine (1 L) and purified by vacuum distillation to afford 4-(1,1,2,3,3-pentamethyl-indan-5-yl)-pyrimidine (200 g) having a boiling point of 153° C. at a pressure of 2.0 mmHg

Aufarbeitung

  1. customA 5 L reaction vessel
  2. temperaturecooled to 25° C
  3. washThe reaction mixture was washed twice with brine (1 L)
  4. distillationpurified by vacuum distillation

Quellen und Nachweise

ORD-Eintrag
ord-390f39fa13a44083bddc8ade61f411a3
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08557876B2

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