Triethylamine → HCID 20306069, Verbindung

HRID 1732400

Reaktionsgleichung

Reaktionsgleichung von HRID 1732400
[C:1]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:6]=[CH:5][C:4]([O:7][CH:8]([N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)[CH:9]([OH:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:3][CH:2]=1.[CH3:26][O:27][CH2:28][N:29]=[C:30]=[O:31].C(N(CC)CC)C.C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>O1CCCC1>[C:1]1([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:6]=[CH:5][C:4]([O:7][CH:8]([N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)[CH:9]([O:14][C:30](=[O:31])[NH:29][CH2:28][O:27][CH3:26])[C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:3][CH:2]=1

Komponenten

6

Edukt 4

HCID 8471TriethylamineHCID 62609Methoxymethyl isocyanateHCID 91656BitertanolHCID 9809426Di-n-butyldilauryltin

Produkt 1

HCID 20306069HCID 20306069, VerbindungAusbeute 82,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

505 g (1.5 moles) of 1-(4-biphenylyloxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol (A form) and 140 g (1.6 moles) of methoxymethyl isocyanate were heated under reflux in 2.5 liters of tetrahydrofuran in the presence of 40 ml of triethylamine and 1 ml of dibutyl-tin dilaurate for 48 hours. Thereafter, the solvent was stripped off in vacuo and 3 liters of petroleum ether were added to the residue. The crystalline precipitate formed was extracted by stirring with 1.5 liters of diisopropyl ether. 528 g (82.5% of theory) of 1-(4-biphenylyloxy)-3,3-dimethyl-2-methoxymethylcarbamoyloxy-1-(1,2,4-triazol-1-yl)-butane (A form) of melting point 95°-98° C. were obtained.

Aufarbeitung

  1. additionwere added to the residue
  2. customThe crystalline precipitate formed
  3. extractionwas extracted

Quellen und Nachweise

ORD-Eintrag
ord-241dca38976241c782d44dc4f4610135
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04237142

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