Stannous Chloride → 3-Chloro-5-hydrazino-phenol

HRID 1517648

Reaktionsgleichung

Reaktionsgleichung von HRID 1517648
[NH2:1][C:2]1[CH:3]=[C:4]([OH:9])[CH:5]=[C:6]([Cl:8])[CH:7]=1.[N:10]([O-])=O.[Na+].[Sn](Cl)Cl.C(=O)([O-])O.[Na+]>Cl.O>[Cl:8][C:6]1[CH:5]=[C:4]([OH:9])[CH:3]=[C:2]([NH:1][NH2:10])[CH:7]=1

Komponenten

7

Edukt 4

HCID 24479Stannous ChlorideHCID 516892Sodium BicarbonateHCID 199869473-Amino-5-chlorophenolHCID 23668193Sodium Nitrite

Produkt 1

HCID 552816153-Chloro-5-hydrazino-phenol

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

2.1 g (14.3 mmol) 3-amino-5-chloro-phenol are dissolved in 20 ml of conc. hydrochloric acid and 20 ml of water and cooled to 0° C. 1.0 g (15.0 mmol) sodium nitrite in 4 ml of water are added. Then a solution of 12.1 g (53.5 mmol) tin(II)-chloride in 16 ml hydrochloric acid is slowly added dropwise at −5° C. It is stirred for 1 hour at 0° C., then adjusted to pH7 with sodium hydrogen carbonate. The precipitate formed is suction filtered and washed with water. The filtrate is extracted with diethyl ether. The organic phase is dried and evaporated to dryness. The residue is extracted with hexane.

Aufarbeitung

  1. customThe precipitate formed
  2. filtrationfiltered
  3. washwashed with water
  4. extractionThe filtrate is extracted with diethyl ether
  5. customThe organic phase is dried
  6. customevaporated to dryness
  7. extractionThe residue is extracted with hexane

Quellen und Nachweise

ORD-Eintrag
ord-f51cbabc9ec145f4b2067317581ab2c5
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08232286B2

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