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Acetic Acid → 5-Cyclohexyl 3-methylamino 4,5,6,7-tetrahydro indazole

HRID 1284013
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1284013
[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=O)[CH:9]([C:14](=S)[NH:15][CH3:16])[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.[NH2:19][NH2:20].C(O)(=O)C.CCOCC>C(O)C>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10]3[NH:20][N:19]=[C:14]([NH:15][CH3:16])[C:9]=3[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 3283Diethyl EtherHCID 24654Hydrazine hydrate (1:1)HCID 215152814-Cyclohexyl 2-methylthiocarbamoyl cyclohexanone

Produkt 1

HCID 215152845-Cyclohexyl 3-methylamino 4,5,6,7-tetrahydro indazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702
Ethanol
Lösungsmittel

Versuchsvorschrift

0.7 g of 4-cyclohexyl 2-methylthiocarbamoyl cyclohexanone dissolved in 30 ml ethanol are added with 0.15 g hydrazine hydrate. The mixture is heated to reflux for 30 mn until the evolution of sulphydric gas has ceased. 0.3 ml acetic acid are thereafter added and the whole is refluxed for 3 hours. The mixture is evaporated off giving a yellow liquid as residue. The residue is taken up with ether; the organic solution is washed with a saturated aqueous solution of sodium bicarbonate then with water until the washings are neutral, finally dried and evaporated off. 0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered and recrystallized from the minimum amount of isopropanol.

Aufarbeitung

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 30 mn until the evolution of sulphydric gas
  3. temperaturethe whole is refluxed for 3 hours
  4. customThe mixture is evaporated off
  5. customgiving a yellow liquid as residue
  6. washthe organic solution is washed with a saturated aqueous solution of sodium bicarbonate
  7. customfinally dried
  8. customevaporated off
  9. custom0.6 g of 5-cyclohexyl 3-methylamino 4,5,6,7-tetrahydroindazole are thus recovered
  10. customrecrystallized from the minimum amount of isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-5c95b3b7eac4496dab84dc969a03bfe7
Quelldatensatz
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03978044

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