Iodine chloride → HCID 86608026, Verbindung

HRID 269078Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 269078
[CH3:1][C:2]1[CH:3]=[C:4]([C:12]2[CH:17]=[C:16]([C:18]([F:21])([F:20])[F:19])[N:15]3[N:22]=[CH:23][CH:24]=[C:14]3[N:13]=2)[CH:5]=[CH:6][C:7]=1[C:8]([F:11])([F:10])[F:9].C([O-])(=O)C.[Na+].[I:30]Cl>C(O)(=O)C.O>[I:30][C:24]1[CH:23]=[N:22][N:15]2[C:16]([C:18]([F:21])([F:19])[F:20])=[CH:17][C:12]([C:4]3[CH:5]=[CH:6][C:7]([C:8]([F:9])([F:10])[F:11])=[C:2]([CH3:1])[CH:3]=3)=[N:13][C:14]=12

Komponenten

6

Edukt 3

HCID 24640Iodine chlorideHCID 517045Sodium AcetateHCID 86608025HCID 86608025, Verbindung

Produkt 1

HCID 86608026HCID 86608026, VerbindungAusbeute 84,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176Acetic AcidLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

To a stirred solution of 5-(3-methyl-4-trifluoromethyl-phenyl)-7-trifluoromethyl-pyrazolo[1,5-a]pyrimidine (2.12 g, 6.14 mmol) in acetic acid (15 ml) was added at room temperature sodium acetate (0.57 g, 6.95 mmol) and drop wise a solution of iodine monochloride (1.13 g, 6.96 mmol) in acetic acid (3.5 ml). The reaction mixture was stirred at room temperature for 16 h, diluted slowly with water (up to 100 ml), stirred at room temperature for 30 min, the precipitate was filtered off, washed with water and dried to give 3-iodo-5-(3-methyl-4-trifluoromethyl-phenyl)-7-trifluoromethyl-pyrazolo[1,5-a]pyrimidine (2.44 g, 84%) as a yellow solid. MS (EI) 471.0 [(M)+]; mp 160° C.

Aufarbeitung

  1. stirringstirred at room temperature for 30 min
  2. filtrationthe precipitate was filtered off
  3. washwashed with water
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-aa1a2a08d13247228faa5d9dee66c37d
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07446113B2

Notizen zur Reaktion

Wird geladen…