6-Chloro-2-benzothiazolamine → N-(6-Chloro-1,3-benzothiazol-2-yl)-N'-ethylurea

HRID 9098

Reaktionsgleichung

Reaktionsgleichung von HRID 9098
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([NH2:9])[S:8][C:4]=2[CH:3]=1.[CH2:12]([N:14]=[C:15]=[O:16])[CH3:13].C(N(CC)CC)C>CN(C=O)C>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[C:7]([NH:9][C:15]([NH:14][CH2:12][CH3:13])=[O:16])[S:8][C:4]=2[CH:3]=1

Komponenten

5

Edukt 3

HCID 72266-Chloro-2-benzothiazolamineHCID 8022Ethyl isocyanateHCID 8471Triethylamine

Produkt 1

HCID 9964976N-(6-Chloro-1,3-benzothiazol-2-yl)-N'-ethylurea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

Three grams of 6-chloro-1,3-benzothiazol-2-amine was dissolved in about 50 mL DMF. Next, about 2.5 mL of EtNCO was added followed by about 3.2 mL of triethylamine. The solution was allowed to react at about 80° C. for about 8 hours. The reaction solvent was then removed in vacuo and the crude oil was taken up in ether. The solids were isolated by filtration and washed with ether. The product was then dried in vacuo. 1H NMR 1.09 (t, 3H, J=7.2 Hz), 3.19 (m, 2H), 6.74 (br s, 1H), 7.37 (d, 1H, J=8.58 Hz), 7.60 (d, 1H, J=8.59 Hz), 8.01 (s, 1H), 10.8 (br s, 1H). LCMS: R.T. 2.3 min, MH-254 m/z.

Aufarbeitung

  1. customto react at about 80° C. for about 8 hours
  2. customThe reaction solvent was then removed in vacuo
  3. customThe solids were isolated by filtration
  4. washwashed with ether
  5. customThe product was then dried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-68f4737b6c484d558c81c99a24e5ed31
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07091227B2

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