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

Hydrochloric Acid → HCID 15615501, Verbindung

HRID 704614
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 704614
[CH:1]([NH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=O.[Cl:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[N:14]=C(S(C)(=O)=O)[N:12]=1.Cl>O1CCCC1.O>[NH:3]([C:1]1[N:12]=[C:11]([Cl:10])[CH:16]=[C:15]([O:17][CH3:18])[N:14]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 7671FormanilideHCID 137292254-Chloro-2-(methanesulfonyl)-6-methoxypyrimidine

Produkt 1

HCID 15615501HCID 15615501, VerbindungAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel
HCID 8028
Tetrahydrofuran
Lösungsmittel

Versuchsvorschrift

1.8 g of formanilide was dissolved in 50 ml of tetrahydrofuran, and 0.4 g of sodium hydride from which the oily matter had been removed beforehand with n-hexane was slowly added to the resulting solution at 10° to 20° C. while cooling with ice water. To the suspension thus obtained was added 3 3 g of 4-chloro-2-methanesulfonyl-6-methoxypyrimidine, and the mixture was stirred for 1 hour at room temperature. Then, 15 ml of 4N hydrochloric acid was added, and reaction was effected for 1 hour under reflux. The reaction liquid was poured in water, extracted with ether, and the ether layer was washed with water, dried over magnesium sulfate, and then the ether was stripped by concentration The residual crystals were recrystallized from n-hexane, and 4.0 g of 2-anilino-4-chloro-6-methoxypyrimidine was obtained (yield 87%). Melting point: 101°-103° C.

Aufarbeitung

  1. custom0.4 g of sodium hydride from which the oily matter had been removed beforehand with n-hexane
  2. additionwas slowly added to the resulting solution at 10° to 20° C.
  3. temperaturewhile cooling with ice water
  4. customTo the suspension thus obtained
  5. customreaction
  6. waitwas effected for 1 hour
  7. temperatureunder reflux
  8. customThe reaction liquid
  9. extractionextracted with ether
  10. washthe ether layer was washed with water
  11. dry with materialdried over magnesium sulfate
  12. concentrationthe ether was stripped by concentration The residual crystals
  13. customwere recrystallized from n-hexane

Quellen und Nachweise

ORD-Eintrag
ord-f8c83e859494465d99a524c2effe22a5
Quelldatensatz
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04988704

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion