5-Bromo-1-methyl-1H-tetrazole → HCID 20403203, Verbindung

HRID 2164744Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2164744
[NH2:1][CH2:2][CH:3]([OH:20])[CH2:4][CH2:5][O:6][C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[CH:8]=1.Br[C:22]1[N:26]([CH3:27])[N:25]=[N:24][N:23]=1>C(O)C>[CH3:27][N:26]1[C:22]([NH:1][CH2:2][CH:3]([OH:20])[CH2:4][CH2:5][O:6][C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([CH2:13][N:14]3[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]3)[CH:8]=2)=[N:23][N:24]=[N:25]1

Komponenten

4

Edukt 2

HCID 127974465-Bromo-1-methyl-1H-tetrazoleHCID 202460151-Amino-4-{3-[(piperidin-1-yl)methyl]phenoxy}butan-2-ol

Produkt 1

HCID 20403203HCID 20403203, VerbindungAusbeute 55,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 1-amino-4-[3-(1-piperidinylmethyl)phenoxy]-2-butanol (1.39 g) and 5-bromo-1-methyl-1H-tetrazole (0.82 g) in absolute ethanol (10 ml) was heated in an autoclave at 125° for 18 h. The solution was evaporated and the residue dissolved in 1M hydrochloric acid (25 ml). The acidic solution was washed with ethyl acetate, basified with excess sodium carbonate and extracted with ethyl acetate. The extract was dried and evaporated to leave a solid which was triturated with dry diethyl ether to give a white solid (1.0 g). This solid was recrystallised from methyl acetate-light petroleum (b.p. 60°-80°) to give the title compound (0.6 g) as white crystals, m.p. 138°-9°.

Aufarbeitung

  1. customThe solution was evaporated
  2. dissolutionthe residue dissolved in 1M hydrochloric acid (25 ml)
  3. washThe acidic solution was washed with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. customThe extract was dried
  6. customevaporated
  7. customto leave a solid which
  8. customwas triturated with dry diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-68a4605673704cfebaac9762fb2aff03
Quelldatensatz
uspto-grants-1985_03
Patentnummer
US04507296

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