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

HRID 26369

Reaktionsgleichung

Reaktionsgleichung von HRID 26369
Cl.[S:2]1[CH:6]=[CH:5][C:4]2[CH:7]([NH2:12])[CH2:8][CH2:9][CH2:10][CH2:11][C:3]1=2.[O-:13][C:14]#[N:15].[K+]>O>[S:2]1[CH:6]=[CH:5][C:4]2[CH:7]([NH:12][C:14]([NH2:15])=[O:13])[CH2:8][CH2:9][CH2:10][CH2:11][C:3]1=2

Komponenten

4

Edukt 2

HCID 11378442Potassium cyanateHCID 213198545,6,7,8-tetrahydro-4H-cyclohepta[b]thiophen-4-amine hydrochloride

Produkt 1

HCID 213198435,6,7,8-tetrahydro-4H-cyclohepta[b]thien-4-ylurea

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

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.

Aufarbeitung

  1. additionAfter completion of the addition
  2. temperaturethe mixture is warmed slowly to 70°-75° C.
  3. temperatureThe mixture is cooled
  4. filtrationthe white solid is collected by filtration
  5. washwashed with water
  6. customThe solid is air-dried
  7. washwashed with acetonitrile
  8. customUpon drying
  9. additionthis crude product is treated with hot acetone whereby there

Quellen und Nachweise

ORD-Eintrag
ord-470edd24cdc84b06b2fd802f9873e6d7
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04150035

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