Reaktion #54647

Reaktionsgleichung

5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophen-4-amine hydrochloride

potassium cyanate

→

5,6,7,8-tetrahydro-4H-cyclohepta[b]thien-4-ylurea

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter completion of the addition
2. 2
   Temperaturthe mixture is warmed slowly to 70°-75° C.
3. 3
   TemperaturThe mixture is cooled
4. 4
   Filtrationthe white solid is collected by filtration
5. 5
   Waschenwashed with water
6. 6
   SonstigeThe solid is air-dried
7. 7
   Waschenwashed with acetonitrile
8. 8
   SonstigeUpon drying
9. 9
   workup.ADDITIONthis crude product is treated with hot acetone whereby there

Vorschrift

A mixture of 50 grams of 5,6,7,8-tetrahydro-4H-cyclohepta[b]thiophen-4-amine hydrochloride in 100 ml. of water is stirred at about 15° C. and a solution of 23.1 grams of potassium cyanate in 100 ml. of water is added dropwise. After completion of the addition, the mixture is warmed slowly to 70°-75° C. and held there for one hour. The mixture is cooled and the white solid is collected by filtration and washed with water. The solid is air-dried, pulverized, and washed with acetonitrile. Upon drying, this crude product is treated with hot acetone whereby there is obtained 5,6,7,8-tetrahydro-4H-cyclohepta[b]thien-4-ylurea, m.p. 217° C. dec.

Quelle