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Hydrazoic acid → 5-(3-Chloropropyl)-1-cyclohexyltetrazole

HRID 1277418
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1277418
[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([NH:7][CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)=O.P(Cl)(Cl)(Cl)(Cl)Cl.[NH:20]=[N+:21]=[N-:22]>C1C=CC=CC=1>[CH:8]1([N:7]2[C:5]([CH2:4][CH2:3][CH2:2][Cl:1])=[N:22][N:21]=[N:20]2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 24530Hydrazoic acidHCID 24819Phosphorus pentachlorideHCID 41034704-chloro-N-cyclohexylbutanamide

Produkt 1

HCID 52099225-(3-Chloropropyl)-1-cyclohexyltetrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel2×

Versuchsvorschrift

Into 200 ml of dried benzene, 30.6 g of N-γ-chlorobutyrylcyclohexylamine was added. While the inside temperature is kept below 20° C. by ice-cooling the outside of the reaction vessel, 30 g of PCl5 was added under stirring condition. After completion of the addition, the stirring is continued for 2 hours at a room temperature, then the reaction mixture is concentrated to a half volume thereof by using an evaporator with a bath temperature of below 50° C. To the concentrated reaction mixture was added dropwise 140 ml of benzene containing 10% of HN3 under stirring condition for 90 minutes while keeping the inside temperature below 15° C. After the addition operation, the reaction mixture is allowed to stand overnight at room temperature. Then the reaction mixture is refluxed for 3 hours with stirring and is concentrated. The thus obtained concentrate is extracted with 200 ml of chloroform. The chloroform layer is washed with 5% NaHCO3 aqueous solution and with water and dried with Na2SO4. After removal of the drying agent, the mother liquor is concentrated and the residue thus obtained is recrystallized from water-containing isopropanol to obtain 28 g of 1-cyclohexyl-5-γ-chloropropyltetrazole in the form of colorless needle like crystals. Melting point: 82°-85° C.

Aufarbeitung

  1. customis kept below 20° C. by ice-
  2. additionwas added
  3. additionAfter completion of the addition
  4. concentrationthe reaction mixture is concentrated to a half volume
  5. customan evaporator with a bath temperature of below 50° C
  6. customTo the concentrated reaction mixture
  7. stirringunder stirring condition for 90 minutes
  8. customthe inside temperature below 15° C
  9. waitto stand overnight at room temperature
  10. temperatureThen the reaction mixture is refluxed for 3 hours
  11. stirringwith stirring
  12. concentrationis concentrated
  13. customThe thus obtained
  14. concentrationconcentrate
  15. extractionis extracted with 200 ml of chloroform
  16. washThe chloroform layer is washed with 5% NaHCO3 aqueous solution and with water
  17. dry with materialdried with Na2SO4
  18. customAfter removal of the drying agent
  19. concentrationthe mother liquor is concentrated
  20. customthe residue thus obtained
  21. customis recrystallized from water-
  22. additioncontaining isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-59dc48467eda4cfc855f4554d627833b
Quelldatensatz
uspto-grants-1981_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04277479

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