Chloroform → HCID 178526560, Verbindung

HRID 79242

Reaktionsgleichung

Reaktionsgleichung von HRID 79242
C([O-])(=O)C.[Na+].[N+:6]([C:9]1[CH:17]=[CH:16][CH:15]=[C:14]2[C:10]=1[CH:11]=[N:12][NH:13]2)([O-:8])=[O:7].C(Cl)(Cl)Cl.[Br:22]Br>C(O)(=O)C>[Br:22][C:11]1[C:10]2[C:14](=[CH:15][CH:16]=[CH:17][C:9]=2[N+:6]([O-:8])=[O:7])[NH:13][N:12]=1

Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 180574-NitroindazoleHCID 24408BromineHCID 517045Sodium Acetate

Produkt 1

HCID 178526560HCID 178526560, VerbindungAusbeute 86,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

Sodium acetate (52.8 g, 644 mmol) and 4-nitro-1H-indazole (100 g, 613 mmol) were mixed with acetic acid (1000 mL) and chloroform (1000 mL) in a 5 L 4-neck flask with mechanical stirring. A solution of bromine (103 g, 644 mmol) in acetic acid (120 mL) was added over approximately 3.5 hours, while keeping the temperature below 21° C. After the addition was completed, the reaction mixture was stirred for an additional 2 hours. The reaction mixture was concentrated under reduced pressure. Water (2000 mL) was added to the residue. The yellow solids were collected by filtration and washed with water (3×1000 mL). The solids were air-dried on the filter and then under vacuum at 40° C. to give the desired product (129 g) as a yellow solid.

Aufarbeitung

  1. customthe temperature below 21° C
  2. additionAfter the addition
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionWater (2000 mL) was added to the residue
  5. filtrationThe yellow solids were collected by filtration
  6. washwashed with water (3×1000 mL)
  7. customThe solids were air-dried on the
  8. filtrationfilter

Quellen und Nachweise

ORD-Eintrag
ord-20188b337dbc41338ecb8a954ab12147
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08841455B2

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