Trimethylamine → HCID 19786006, Verbindung

HRID 256749

Reaktionsgleichung

Reaktionsgleichung von HRID 256749
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.C(Cl)Cl.CN(C)C.Cl[C:24]([O:26][CH2:27][C:28]#[CH:29])=[O:25]>C(Cl)Cl.O>[CH2:27]([O:26][C:24]([O:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([O:15][C:24]([O:26][CH2:27][C:28]#[CH:29])=[O:25])=[CH:11][CH:10]=2)=[CH:6][CH:7]=1)=[O:25])[C:28]#[CH:29]

Komponenten

6

Edukt 4

HCID 1146TrimethylamineHCID 6344DichloromethaneHCID 12111Bis(4-hydroxyphenyl)methaneHCID 3356829Propargyl chloroformate

Produkt 1

HCID 19786006HCID 19786006, VerbindungAusbeute 93,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 21908982Water methylene chlorideLösungsmittel

Versuchsvorschrift

A flask equipped with a stirrer, thermometer, nitrogen gas tube and reflux condenser was charged with 20.0 g of bis(4-hydroxyphenyl)methane, 50.0 g of methylene chloride and 23.0 g of trimethylamine. To the flask was added 26.0 g of propargyl chloroformate dropwise over one hour and the mixture was allowed to react for 6 hours at 30° C. After the reaction, the reaction mixture was treated with methylene chloride-water mixture and the organic phase was separated followed by drying over magnesium sulfate overnight. After filtering, the filtrate was evaporated in a rotary evaporator. The resulting crystals were recrystallized to give the title compound melting at 60° C. at a yield of 93.6% of theory.

Aufarbeitung

  1. customA flask equipped with a stirrer
  2. temperaturethermometer, nitrogen gas tube and reflux condenser
  3. customto react for 6 hours at 30° C
  4. customAfter the reaction
  5. customthe organic phase was separated
  6. dry with materialby drying over magnesium sulfate overnight
  7. filtrationAfter filtering
  8. customthe filtrate was evaporated in a rotary evaporator
  9. customThe resulting crystals were recrystallized

Quellen und Nachweise

ORD-Eintrag
ord-3871fff872f44c6e9f669129342353af
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05258542

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