Dicyclohexylamine → HCID 22117430, Verbindung

HRID 1275626Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1275626
[CH3:1][C:2]1[C:3]([S:16][C:17]2[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[CH:19][CH:18]=2)=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.C1(NC2CCCCC2)CCCCC1.S(Cl)([Cl:41])=O>ClCCl>[CH3:1][C:2]1[C:3]([S:16][C:17]2[CH:25]=[CH:24][C:20]([C:21]([Cl:41])=[O:22])=[CH:19][CH:18]=2)=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1

Komponenten

5

Edukt 3

HCID 7582DicyclohexylamineHCID 24386Thionyl ChlorideHCID 30259184-[(3,5,5,8,8-Pentamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)sulfanyl]benzoic acid

Produkt 1

HCID 22117430HCID 22117430, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 1.4 g (4 mmol) of 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylthio)benzoic acid in 100 ml of anhydrous dichloromethane was introduced into a round-bottomed flask, 900 μl (4.4 mmol) of dicyclohexylamine were added and the mixture was stirred for one hour. Next, 320 μl (4.4 mmol) of thionyl chloride were added and the mixture was stirred for one hour. The reaction medium was evaporated to dryness, taken up in anhydrous ethyl ether, the dicyclohexylamine salt filtered off and the filtrate evaporated. 1.5 g (100%) of the crude acid chloride was recovered which was used as such in the continuation of the synthesis to follow.

Aufarbeitung

  1. stirringthe mixture was stirred for one hour
  2. customThe reaction medium was evaporated to dryness
  3. filtrationthe dicyclohexylamine salt filtered off
  4. customthe filtrate evaporated
  5. custom1.5 g (100%) of the crude acid chloride was recovered which
  6. customsuch in the continuation of the synthesis

Quellen und Nachweise

ORD-Eintrag
ord-f37de56e665c40b78509ecc73a9a5c87
Quelldatensatz
uspto-grants-2000_12
Patentnummer
US06162815

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