Sodium borohydride → HCID 70434749, Verbindung

HRID 355200Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 355200
O.[Cl:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([Cl:10])=[CH:5][C:4]=1[C:11]([CH:13]=O)=[O:12].[NH2:15][C:16]([CH3:29])([CH3:28])[CH2:17][CH2:18][N:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]=[CH:20]1.[BH4-].[Na+]>CO>[ClH:2].[ClH:2].[Cl:2][C:3]1[CH:8]=[C:7]([OH:9])[C:6]([Cl:10])=[CH:5][C:4]=1[CH:11]([OH:12])[CH2:13][NH:15][C:16]([CH3:29])([CH2:17][CH2:18][N:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[N:21]=[CH:20]1)[CH3:28]

Komponenten

5

Edukt 3

HCID 4311764Sodium borohydride2×HCID 20214926HCID 20214926, VerbindungHCID 20214946HCID 20214946, Verbindung

Produkt 1

HCID 70434749HCID 70434749, VerbindungAusbeute 50,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 9.3 gm of 2,5-dichloro-4-hydroxyphenylglyoxal hydrate, 7.25 gm of 1-(3-amino-3-methylbutyl)-benzimidazole and 100 ml of alcohol was stirred for 3 hours at 40°-45° C. The resulting solution was subsequently cooled, admixed in portions with 8 gm of sodium borohydride, and the mixture was stirred for 3 hours at room temperature. After the addition of 100 ml of methanol for decomposition of the sodium borohydride, the mixture was allowed to stand for 10 hours, the solvent was distilled off under reduced pressure, the residue was dissolved in 200 ml of water, and the solution was acidified with concentrated hydrochloric acid. 9.5 gm of 1-(2,5-dichloro-4-hydroxyphenyl)-2-[4-(1-benzimidazolyl)-2-methyl-2-butylamino]-ethanol dihydrochloride×1 H2O, m.p. 180°-183° C., of the formula ##STR33## were obtained. The yield was 50.4% of theory.

Aufarbeitung

  1. temperatureThe resulting solution was subsequently cooled
  2. stirringthe mixture was stirred for 3 hours at room temperature
  3. waitto stand for 10 hours
  4. distillationthe solvent was distilled off under reduced pressure
  5. dissolutionthe residue was dissolved in 200 ml of water
  6. customwere obtained

Quellen und Nachweise

ORD-Eintrag
ord-2edd5ff5e4e34511bc7a7bf869ab5ac1
Quelldatensatz
uspto-grants-1983_03
Patentnummer
US04378361

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