Phosphoric Acid → HCID 86722238, Verbindung

HRID 869389Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 869389
[NH2:1][C:2]1[C:6]2[C:7]([Cl:13])=[C:8]([O:11][CH3:12])[CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:14](=[O:25])/[CH:15]=[CH:16]/[C:17]1[S:21][C:20]([CH:22]([CH3:24])[CH3:23])=[N:19][CH:18]=1.CC#N.OP(O)(O)=O>[Cl-].[Cl-].[Zn+2].CC(O)=O>[Cl:13][C:7]1[C:6]2[C:2]3[NH:1][CH:16]([C:17]4[S:21][C:20]([CH:22]([CH3:23])[CH3:24])=[N:19][CH:18]=4)[CH2:15][C:14](=[O:25])[C:3]=3[O:4][C:5]=2[CH:10]=[CH:9][C:8]=1[O:11][CH3:12]

Komponenten

6

Edukt 3

HCID 1004Phosphoric AcidHCID 6342AcetonitrileHCID 86722237HCID 86722237, Verbindung

Produkt 1

HCID 86722238HCID 86722238, VerbindungAusbeute 68,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 3007855ZincchlorideKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

9A (3.5 g, 9.28 mmol) was added to MeCN (50 mL) and stirred at room temperature. To the mixture was added ZnCl2 (1.91 g, 13.93 mmol, 1.5 eq), followed by AcOH (50 mL) and H3PO4 (50 mL) The reaction mixture was heated to 80° C. and stirred overnight. After reaction completed, the mixture was cooled and poured into crushed ice under stirring, neutralized to pH=7˜8, extracted with ethyl acetate, dried and concentrated to give 2.4 g of product (9B).

Aufarbeitung

  1. temperaturewas heated to 80° C.
  2. stirringstirred overnight
  3. customAfter reaction
  4. temperaturethe mixture was cooled
  5. additionpoured
  6. custominto crushed ice
  7. stirringunder stirring
  8. extractionextracted with ethyl acetate
  9. customdried
  10. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-cb3a3555d48746bb9b7a6c3cb05bee96
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08969373B2

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