Water → HCID 21474500, Verbindung

HRID 274027

Reaktionsgleichung

Reaktionsgleichung von HRID 274027
[SH:1][CH2:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=1.C(N(CC)CC)C.[CH3:19][C:20]1([CH3:35])[CH2:29][CH2:28][C:27]([CH3:31])([CH3:30])[C:26]2[CH:25]=[C:24]([C:32](Cl)=[O:33])[CH:23]=[CH:22][C:21]1=2.O>C1COCC1.CCCCCC.C(OCC)C>[CH3:19][C:20]1([CH3:35])[CH2:29][CH2:28][C:27]([CH3:30])([CH3:31])[C:26]2[CH:25]=[C:24]([C:32]([S:1][CH2:2][C:3]3[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][CH:4]=3)=[O:33])[CH:23]=[CH:22][C:21]1=2

Komponenten

8

Edukt 4

HCID 962WaterHCID 8471TriethylamineHCID 5850394-(Mercaptomethyl)benzoic acidHCID 27954665,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carbonyl chloride

Produkt 1

HCID 21474500HCID 21474500, VerbindungAusbeute 66 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 3283Diethyl EtherLösungsmittelHCID 8028TetrahydrofuranLösungsmittel2×HCID 8058HexaneLösungsmittel

Versuchsvorschrift

1.68 g (10 mmol) of 4-mercaptomethylbenzoic acid, 2.8 ml (20 mmol) of triethylamine and 50 ml of THF are introduced into a round-bottomed flask. A solution of 2.5 g (10 mmol) of 5,6,7,8-tetrahydro-5,5,8,8-tetramethyl- 2-naphthoyl chloride in 50 ml of THF is added dropwise and the mixture is stirred at room temperature for four hours. The reaction medium is poured into water, the mixture is extracted with ethyl ether and the organic phase is separated after settling has taken place, then dried over magnesium sulphate and evaporated. The residue obtained is ground in 50 ml of a mixture of ethyl ether and hexane (50:50) and then filtered off. 2.5 g (66%) of the expected acid, melting point 150°-151° C., are obtained.

Aufarbeitung

  1. extractionthe mixture is extracted with ethyl ether
  2. customthe organic phase is separated after settling
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customThe residue obtained
  6. filtrationfiltered off

Quellen und Nachweise

ORD-Eintrag
ord-828056ae12e341198463f0990e65d56d
Quelldatensatz
uspto-grants-1995_02
Patentnummer
US05387594

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