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

HRID 1042060

Reaktionsgleichung

Reaktionsgleichung von HRID 1042060
[CH3:1][C:2]([C:4]1[CH:5]=[C:6]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH3:14])([CH3:13])[CH:8]([CH3:15])[C:7]2([CH3:17])[CH3:16])=O.[C:18](O)(=O)C.[CH:22]([NH2:24])=[NH:23]>C(O)CCC>[CH3:13][C:9]1([CH3:14])[C:10]2[C:6](=[CH:5][C:4]([C:2]3[CH:1]=[CH:18][N:24]=[CH:22][N:23]=3)=[CH:12][CH:11]=2)[C:7]([CH3:17])([CH3:16])[CH:8]1[CH3:15]

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 1,1,2,3,3-pentamethyl-5-indanyl methyl ketone (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-(2,3-dihydro-1,1,2,3,3-pentamethyl-1H-inden-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-1157e877928647cd92eeac383cb20a76
Quelldatensatz
uspto-grants-2013_10
Patentnummer
US08557827B2

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