Sodium borohydride → HCID 55036, Verbindung

HRID 2417617Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2417617
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:27])[CH2:12][N:13]2[CH2:18][CH2:17][N:16]([C:19]3[C:20](=[O:26])[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=3)[CH2:15][CH2:14]2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[BH4-].[Na+]>CO.C(Cl)(Cl)Cl>[OH:27][CH:11]([C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)[CH2:12][N:13]1[CH2:18][CH2:17][N:16]([C:19]2[C:20](=[O:26])[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:15][CH2:14]1

Komponenten

5

Edukt 2

HCID 4311764Sodium borohydrideHCID 13298561HCID 13298561, Verbindung

Produkt 1

HCID 55036HCID 55036, VerbindungAusbeute 99,5 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

To a solution of 2-[4-[2-(3,4-dimethoxyphenyl)-2-oxoethyl]-1-piperazinyl]-2,4,6-cycloheptatrien-1-one (1.33 g, described above) in methanol (20 ml) and chloroform (5 ml), sodium borohydride (0.31 g) was added portionwise over a period of one hr. The solvent was then removed under vacuum. The residue was taken up in chloroform, washed with water, ammonium chloride solution followed by water, dried and evaporated to give the title compound (1.33 g): mp 122°-124° C.; ir(CHCl3) 3420, 1565, 1260 and 1140 cm-1 ; uv max(MeOH) 352 (ε=10040), 256 (ε=15660) and 227 nm (ε=20250); nmr(CDCl3) δ2.6 (m, 6H), 3.3 (m, 4H), 3.85 (s, 6H), 4.7 (m,1H) and 6.8 (m,6H); and Anal. Calcd for C21H26N2O4 : C, 68.08% H, 7.08% N, 7.56% and Found: C, 67.78% H, 7.06% N, 7.36%.

Aufarbeitung

  1. customThe solvent was then removed under vacuum
  2. washwashed with water, ammonium chloride solution
  3. customdried
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-c7fb2629372847f18e853da843972340
Quelldatensatz
uspto-grants-1984_09
Patentnummer
US04469695

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