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Hydrochloric Acid → HCID 178423709, Verbindung

HRID 363746
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 363746
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)#[N:2].C([N:18](CC)CC)C.S.[NH2:24][NH2:25].N([O-])=O.[Na+].Cl>C(O)C>[NH:24]1[C:1]([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[C:9]2[CH:10]=[CH:11][C:12]([CH3:15])=[CH:13][CH:14]=2)=[N:2][N:18]=[N:25]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 6

HCID 313Hydrochloric AcidHCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 9321HydrazineHCID 1455122-Cyano-4'-methylbiphenylHCID 23668193Sodium Nitrite

Produkt 1

HCID 178423709
HCID 178423709, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

First, 26.9 mmol of 2-cyano-4'-methyl-1,1'-biphenyl was dissolved in 150 ml of ethanol, and 53.9 mmol of triethylamine and 105 mmol of hydrogen sulfide were added to the solution at room temperature, followed by adding 134.5 mmol of anhydrous hydrazine and keeping at the reflux temperature for 48 hours. The reaction mixture was warmed. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in 100 ml of ethanol added thereto, and 108 mmol of sodium nitrite and 100 ml of concentrated hydrochloric acid was added at 0° C. After keeping at 0°-5° C. for 2 hours, the reaction mixture was extracted with ethyl acetate to give 2-(tetrazol-5-yl)-4'-methyl-1,1'-biphenyl. Yield, 52%

Aufarbeitung

  1. temperatureThe reaction mixture was warmed
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionThe residue was dissolved in 100 ml of ethanol
  4. additionadded
  5. waitAfter keeping at 0°-5° C. for 2 hours
  6. extractionthe reaction mixture was extracted with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-b65ec69013b448d88aa738415440cbdc
Quelldatensatz
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05874593

Notizen zur Reaktion

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