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Hydrochloric Acid → HCID 19962752, Verbindung

HRID 52013
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 52013
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[N:6]=[C:5]([O:11][C:12]2[CH:20]=[CH:19][C:18]3[NH:17][C:16]([CH3:21])=[C:15]([N+:22]([O-])=O)[C:14]=3[C:13]=2[C:25]([O:27][CH2:28][CH:29]=[CH2:30])=[O:26])[N:4]=1.Cl.[Sn]>CO>[NH2:22][C:15]1[C:14]2[C:13]([C:25]([O:27][CH2:28][CH:29]=[CH2:30])=[O:26])=[C:12]([O:11][C:5]3[N:6]=[C:7]([O:9][CH3:10])[CH:8]=[C:3]([O:2][CH3:1])[N:4]=3)[CH:20]=[CH:19][C:18]=2[NH:17][C:16]=1[CH3:21]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 5352426Tin atomHCID 19962765HCID 19962765, Verbindung

Produkt 1

HCID 19962752HCID 19962752, VerbindungAusbeute 79,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

3.4 g of allyl 5-[(4,6-dimethoxypyrimidin-2-yl)oxy]-2-methyl-3-nitroindol-4-carboxylate was dissolved in 50 ml of methanol, and 5 ml of concentrated hydrochloric acid was added thereto. Then, 4.9 g of tin powder was gradually added at room temperature. Them, the mixture was stirred at room temperature for 12 hours. The solid was filtered off, and then residue was concentrated under reduced pressure and extracted with ethyl acetate. The organic layer was washed with water and then dried over anhydrous sodium sulfate. The residue obtained by concentration under reduced pressure, was crystallized from isopropyl ether to obtain 2.5 g (yield: 79%) of the desired product. mp: 132°-135° C.

Aufarbeitung

  1. filtrationThe solid was filtered off
  2. concentrationresidue was concentrated under reduced pressure
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe residue obtained by concentration under reduced pressure
  7. customwas crystallized from isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-172b663c480f428491802387607eff65
Quelldatensatz
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05616537

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