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Dimethylamine → N,N-Dimethyl-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazin-6-amine

HRID 1980088
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1980088
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=1.[CH3:15][NH:16][CH3:17]>CO>[CH3:15][N:16]([CH3:17])[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[N:14][N:4]2[N:3]=1
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Komponenten

4

Edukt 2

HCID 674DimethylamineHCID 133767996-Chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine

Produkt 1

HCID 13376800N,N-Dimethyl-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazin-6-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture was prepared from 6 g of 6-chloro-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine, 150 ml of methanol and 125 ml of 40% aqueous dimethylamine. This mixture was heated at reflux for 3 hours and then cooled. The precipitate which formed was separated by filtration and partitioned between methylene chloride and water. The organic layer was separated, dried over sodium sulfate, and concentrated to leave a residual solid. This was recrystallized from ethanol to give 6-dimethylamino-7,8,9,10-tetrahydrotetrazolo[5,1-a]phthalazine melting at about 239°-240° C.

Aufarbeitung

  1. temperatureThis mixture was heated
  2. temperatureat reflux for 3 hours
  3. temperaturecooled
  4. customThe precipitate which formed
  5. customwas separated by filtration
  6. custompartitioned between methylene chloride and water
  7. customThe organic layer was separated
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated
  10. customto leave a residual solid
  11. customThis was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-df05722a5b8544f08714fcde3ed78591
Quelldatensatz
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04485106

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