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Carbon Disulfide → HCID 13302038, Verbindung

HRID 620071
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 620071
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:4]=[C:5]([CH2:9][C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[O:11])[CH:6]=[CH:7][CH:8]=1.[C:23](=[S:25])=[S:24].[OH-].[K+].Cl[CH2:29][CH2:30][CH2:31]Cl>CS(C)=O.O.CCCCCC>[S:24]1[CH2:31][CH2:30][CH2:29][S:25][C:23]1=[C:9]([C:5]1[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:21])([F:22])[F:1])[CH:4]=1)[C:10]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])=[O:11]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 6348Carbon DisulfideHCID 88811,3-DichloropropaneHCID 14797Potassium HydroxideHCID 13302037Octyl [3-(trifluoromethyl)phenyl]acetate

Produkt 1

HCID 13302038HCID 13302038, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 679
Dimethyl Sulfoxide
Lösungsmittel
HCID 962WaterLösungsmittel2×
HCID 8058HexaneLösungsmittel

Versuchsvorschrift

To a solution of n-octyl 3-trifluoromethylphenylacetate (112.2 g) in dimethyl sulphoxide (850 ml) there are added carbon disulphide (30.4 g) and, slowly, a solution of potassium hydroxide (60.0 g) in water (100 ml). The mixture is stirred for 2 hours at 40°. 1,3-dichloropropane (40.1 g) is then added and the mixture is stirred at 50° for 3 hours. Water (800 ml) and hexane (800 ml) are added, the two phases are separated and the aqueous solution is extracted with hexane (2×500 ml). The combined organic phases are washed with water (400 ml), dried over magnesium sulphate and evaporated. The residue is crystallized from pentane. The product is dried in vacuo to constant weight to yield n-octyl (1,3-dithian-2-ylidene)-(3-trifluoromethylphenyl)-acetate, m.p. 49° (as Example 11).

Aufarbeitung

  1. stirringthe mixture is stirred at 50° for 3 hours
  2. customthe two phases are separated
  3. extractionthe aqueous solution is extracted with hexane (2×500 ml)
  4. washThe combined organic phases are washed with water (400 ml)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated
  7. customThe residue is crystallized from pentane
  8. customThe product is dried in vacuo to constant weight

Quellen und Nachweise

ORD-Eintrag
ord-9cbdcc59e38a4bb29c849cc2de21e66c
Quelldatensatz
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04818765

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