Cyanogen Bromide → HCID 69373404, Verbindung

HRID 1372474Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1372474
[N:1]#[C:2]Br.[I:4][C:5]1[CH:6]=[C:7]([CH:12]=[CH:13][CH:14]=1)[C:8]([NH:10]N)=[O:9].[OH-].[NH4+:16]>CO>[NH2:16][N:1]1[CH2:2][N:10]=[C:8]([C:7]2[CH:12]=[CH:13][CH:14]=[C:5]([I:4])[CH:6]=2)[O:9]1

Komponenten

5

Edukt 3

HCID 10476Cyanogen BromideHCID 14923Ammonium HydroxideHCID 6157743-Iodobenzohydrazide2×

Produkt 1

HCID 69373404HCID 69373404, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

A solution of cyanogen bromide (1.06 g, 10.0 mmol) in 10 mL of methanol was added dropwise to an ice-cold suspension of 3-iodobenzhydrazide (2.62 g, 10.0 mmol, Intermediate 7, Step A) in 20 mL of methanol. After 30 min, the mixture was allowed to warm to room temperature and was then warmed at reflux for 1.5 h. The resultant solution was cooled to 0° C., and neutralized to pH 9 with concentrated aqueous ammonium hydroxide. The resultant precipitate was collected, washed with methanol, and dried in vacuo to afford the product as an off-white powder. LC/MS 288.0 (M+1).

Aufarbeitung

  1. temperaturewas then warmed
  2. temperatureat reflux for 1.5 h
  3. customThe resultant precipitate was collected
  4. washwashed with methanol
  5. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-5eb302d548784ab4b320fcfecb51b6d9
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07157490B2

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