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Potassium Phosphate, Tribasic → HCID 90308924, Verbindung

HRID 2283705
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2283705
[CH:1]1(B(O)O)[CH2:3][CH2:2]1.F[B-](F)(F)F.C1(P(C2CCCCC2)C2CCCCC2)CCCCC1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].Br[C:40]1[C:48]2[C:44](=[CH:45][N:46]([CH3:49])[N:47]=2)[CH:43]=[C:42]([N+:50]([O-:52])=[O:51])[CH:41]=1>C1(C)C=CC=CC=1.O.C([O-])(=O)C.[Cu+2].C([O-])(=O)C>[CH:1]1([C:40]2[C:48]3[C:44](=[CH:45][N:46]([CH3:49])[N:47]=3)[CH:43]=[C:42]([N+:50]([O-:52])=[O:51])[CH:41]=2)[CH2:3][CH2:2]1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 62657Potassium Phosphate, TribasicHCID 2760897Cyclopropylboronic acidHCID 20066521Tri(cyclohexyl)phosphine tetrafluoroborateHCID 90308679HCID 90308679, Verbindung

Produkt 1

HCID 90308924HCID 90308924, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 8895
Cupric acetate
Katalysator
HCID 962WaterLösungsmittel
HCID 1140TolueneLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A solution of cyclopropyl boronic acid (347 mg), palladium acetate (II) (31 mg), tricyclohexylphosphine tetrafluoroborate (99 mg), and potassium phosphate (1 g) in toluene (20 mL) and water (1 mL) was added to 7-bromo-2-methyl-5-nitro-2H-indazole obtained in Example 65 (Step 1) (361 mg), and the reaction solution was stirred at 100° C. for 11 hours. After dilution with ethyl acetate, the reaction solution was washed successively with water and a saturated saline solution. After drying over anhydrous sodium sulfate, the solvent was evaporated under vacuum. The resultant residue was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate) to obtain 7-cyclopropyl-2-methyl-5-nitro-2H-indazole.

Aufarbeitung

  1. washAfter dilution with ethyl acetate, the reaction solution was washed successively with water
  2. dry with materialAfter drying over anhydrous sodium sulfate
  3. customthe solvent was evaporated under vacuum
  4. customThe resultant residue was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-c23eaa132b5f496c9407e3b22da302ac
Quelldatensatz
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09145414B2

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