Propionic Acid → HCID 70613469, Verbindung

HRID 2083751

Reaktionsgleichung

Reaktionsgleichung von HRID 2083751
[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]([CH:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)(O)[C:4]=2[CH:3]=1.S(C1C=CC=CC=1[C:30]([O:32]C(=O)C1C=CC=CC=1S(O)(=O)=O)=[O:31])(O)(=O)=O.[C:49]([OH:53])(=[O:52])[CH2:50][CH3:51].[OH-].[Na+]>O>[C:30]([OH:32])(=[O:31])/[CH:51]=[CH:50]\[C:49]([OH:53])=[O:52].[Cl:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5](=[C:17]3[CH2:22][CH2:21][N:20]([CH3:23])[CH2:19][CH2:18]3)[C:4]=2[CH:3]=1

Komponenten

6

Edukt 4

HCID 1032Propionic AcidHCID 14798Sodium HydroxideHCID 118096639H-Xanthen-9-ol, 2-chloro-9-(1-methyl-4-piperidinyl)-HCID 13795534Sulphobenzoic anhydride

Produkt 1

HCID 70613469HCID 70613469, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 12.5 g. (0.038 m.) of the xanthene-9-ol, 14.0 g. (0.76 m.) of o-sulfobenzoic anhydride and 380 ml. of propionic acid is refluxed for three hours. The reaction mixture is heated in vacuo at 100° C. and the resulting syrup is dissolved in water, made strongly basic with 40% sodium hydroxide solution, extracted with ether, and the dried extract is evaporated. The residual free base is dissolved in ethyl acetate and maleic acid (4.4 g.) is added to yield 4-(2-chloro-9-xanthenylidene)-1-methylpiperidine maleate, m.p. 206°-207° C.

Aufarbeitung

  1. additionA mixture of 12.5 g
  2. extractionextracted with ether
  3. extractionthe dried extract
  4. customis evaporated
  5. dissolutionThe residual free base is dissolved in ethyl acetate
  6. additionmaleic acid (4.4 g.) is added

Quellen und Nachweise

ORD-Eintrag
ord-2c4b050a73984c9c8316ee23d073ec72
Quelldatensatz
uspto-grants-1978_04
Patentnummer
US04086350

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