Ethyl Acetate → 7-Amino-4-chloro-6-fluoro-2-methylbenzothiazole

HRID 1419711Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1419711
[Cl:1][C:2]1[C:7]2[N:8]=[C:9]([CH3:11])[S:10][C:6]=2[C:5]([N+:12]([O-])=O)=[C:4]([F:15])[CH:3]=1.C(OCC)(=O)C>O.Cl.[Fe]>[NH2:12][C:5]1[C:6]2[S:10][C:9]([CH3:11])=[N:8][C:7]=2[C:2]([Cl:1])=[CH:3][C:4]=1[F:15]

Komponenten

6

Edukt 2

HCID 8857Ethyl AcetateHCID 537041054-Chloro-6-fluoro-2-methyl-7-nitrobenzothiazole

Produkt 1

HCID 537099237-Amino-4-chloro-6-fluoro-2-methylbenzothiazole

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23925IronKatalysatorHCID 313Hydrochloric AcidLösungsmittelHCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

6 g of iron powder were added to a suspension of 8 g (32 mmol) of 4-chloro-6-fluoro-2-methyl-7-nitrobenzothiazole in 100 ml of water and 9 ml of concentrated hydrochloric acid, which suspension had been heated to 80° C., after which the mixture was refluxed for 3 hours. 200 ml of ethyl acetate were then added to the reaction mixture. The solid was filtered off. The remaining organic phase was washed with water, dried over magnesium sulfate and finally evaporated down. Yield: 4.5 g.

Aufarbeitung

  1. temperatureafter which the mixture was refluxed for 3 hours
  2. filtrationThe solid was filtered off
  3. washThe remaining organic phase was washed with water
  4. dry with materialdried over magnesium sulfate
  5. customfinally evaporated down

Quellen und Nachweise

ORD-Eintrag
ord-37de1006222e41ceac0e5112e086f55f
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05888940

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