Propargyl bromide → 2-Propynylpiperazine

HRID 437824Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 437824
C(=O)([O-])[O-].[Na+].[Na+].COC1C=CC2CC([N:19]3[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]3)C3C=C(C)C=CC=3OC=2C=1.[CH2:31](Br)[C:32]#[CH:33]>C(O)CCC>[C:31]([CH:21]1[CH2:20][NH:19][CH2:24][CH2:23][NH:22]1)#[C:32][CH3:33]

Komponenten

5

Edukt 3

HCID 7842Propargyl bromideHCID 10340Sodium CarbonateHCID 227679281-[10,11-Dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-piperazine

Produkt 1

HCID 665838092-Propynylpiperazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 2631-ButanolLösungsmittel2×

Versuchsvorschrift

3.8 G. of sodium carbonate are added to a solution of 10 g. of 1-[10,11 -dihydro-3-methoxy-8-methyl-dibenz[b,f]oxepin-10-yl]-piperazine in 55 ml. of butanol and then a solution of 2.5 ml. of propargyl bromide in 20 ml. of butanol is added dropwise. Then, the mixture is stirred for 20 hours at room temperature and the solvent is removed by distillation under reduced pressure. After working-up in an analogous manner to that described in Example 13, there is isolated crude 1-[10,11-dihydro-3-methoxy-8-methyl-dibenz[ b,f]oxepin-10-yl]-4-(2-propynylpiperazine in the form of an oil. The dihydrochloride, prepared in ethanol and recrystallized from methanol/ether, melts at 210°-212° C. (with decomposition).

Aufarbeitung

  1. customthe solvent is removed by distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-66ef0b4ead964a0f92737c82963b791c
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04032525

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