Sulfuric Acid → 5-Nitro-1,3-benzothiazol-2-amine

HRID 1383059Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1383059
Cl[C:2]1[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=1[NH2:4].O.O.O.[S-2].[Na+].[Na+].S(=O)(=O)(O)O.[NH2:23][C:24](N)=[S:25].NC1C=C([N+]([O-])=O)C=CC=1S>CCCCOCCO.CO.O>[NH2:23][C:24]1[S:25][C:2]2[CH:8]=[CH:7][C:6]([N+:9]([O-:11])=[O:10])=[CH:5][C:3]=2[N:4]=1

Komponenten

9

Edukt 5

HCID 1118Sulfuric AcidHCID 226912-Chloro-5-nitroanilineHCID 2723790ThioureaHCID 63364002-Amino-4-nitrobenzenethiolHCID 24846073Sodium sulphide trihydrate

Produkt 1

HCID 27547595-Nitro-1,3-benzothiazol-2-amine

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 887MethanolLösungsmittelHCID 962WaterLösungsmittelHCID 81332-ButoxyethanolLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A solution of 8.63 g of 2-chloro-5-nitroaniline and 9.9 g of sodium sulphide trihydrate in 80 ml of butyl glycol was stirred at 80° C. for 30 minutes. After adding 4.16 ml of concentrated sulphuric acid, 7.6 g of thiourea were added to the 2-amino-4-nitrothiophenol, and the mixture was stirred at 120° C. for 3 hours. The reaction mixture was discharged into 400 ml of water and 50 ml of methanol, and the solid was filtered off with suction and washed with water. 5.4 g of crude 2-amino-5-nitrobenzothiazole, the identity of which was confirmed by TLC comparison with authentic material, were obtained.

Aufarbeitung

  1. filtrationthe solid was filtered off with suction
  2. washwashed with water
  3. customwere obtained

Quellen und Nachweise

ORD-Eintrag
ord-a2191bc50d554de38efb714c914150a2
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04808723

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