StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

(Methylthio)acetic acid → N-[2-chloro-4-[5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]phenyl]methyl-2-(methylthio) acetamide

HRID 1880237
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1880237
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH2:13][C:12]([C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[C:20]([Cl:26])[CH:19]=3)([C:14]([F:17])([F:16])[F:15])[O:11][N:10]=2)=[CH:5][C:4]=1[Cl:27].[CH3:28][S:29][CH2:30][C:31](O)=[O:32].Cl.CN(C)CCCN=C=NCC.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl.C(N(CC)CC)C>[Cl:27][C:4]1[CH:5]=[C:6]([C:9]2[CH2:13][C:12]([C:18]3[CH:23]=[C:22]([Cl:24])[C:21]([Cl:25])=[C:20]([Cl:26])[CH:19]=3)([C:14]([F:17])([F:16])[F:15])[O:11][N:10]=2)[CH:7]=[CH:8][C:3]=1[CH2:2][NH:1][C:31](=[O:32])[CH2:30][S:29][CH3:28]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 75551(Methylthio)acetic acidHCID 516892Sodium BicarbonateHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 446282993-(4-Aminomethyl-3-chlorophenyl)-5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole

Produkt 1

HCID 49763421
N-[2-chloro-4-[5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole-3-yl]phenyl]methyl-2-(methylthio) acetamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

To a solution of 0.11 g of 3-(4-aminomethyl-3-chlorophenyl)-5-(3,4,5-trichlorophenyl)-5-trifluoromethyl-4,5-dihydroisoxazole, 0.051 g of (methylthio) acetic acid and 0.048 g of triethylamine in 2 mL of chloroform, 0.092 g of 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride was added and the resultant mixture was stirred at room temperature for 15 hours. After the completion of the reaction, 2 mL of a saturated sodium hydrogen carbonate aqueous solution was added to the reaction mixture and the organic phase was separated off, followed by purifying the organic phase as it was by preparative medium pressure liquid chromatography eluting with ethyl acetate-hexane (a gradient from 1:4 to 1:1) using a medium pressure preparative apparatus (trade name: YFLC-Wprep; manufactured by Yamazen Corporation) to obtain 0.12 g of the objective substance as a colorless resinoid.

Aufarbeitung

  1. additionwas added to the reaction mixture
  2. customthe organic phase was separated off
  3. customby purifying the organic phase as it
  4. washeluting with ethyl acetate-hexane (a gradient from 1:4 to 1:1)
  5. customto obtain 0.12 g of the objective substance as a colorless resinoid

Quellen und Nachweise

ORD-Eintrag
ord-94d6b82d4c6747d9aab98e30b239e20e
Quelldatensatz
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08318757B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion