3-(Chloromethyl)pyridine → HCID 22320205, Verbindung

HRID 498005

Reaktionsgleichung

Reaktionsgleichung von HRID 498005
O=[C:2]([CH3:15])[CH2:3][C:4]1[O:9][C:8](=[O:10])[C:7]2[CH:11]=[CH:12][CH:13]=[CH:14][C:6]=2[N:5]=1.[NH:16]([CH2:18][C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)[NH2:17].ClCC1C=NC=CC=1>C(O)C>[CH3:15][C:2]1[CH:3]=[C:4]([NH:5][C:6]2[CH:14]=[CH:13][CH:12]=[CH:11][C:7]=2[C:8]([OH:9])=[O:10])[N:16]([CH2:18][C:19]2[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=2)[N:17]=1

Komponenten

5

Edukt 3

HCID 183583-(Chloromethyl)pyridineHCID 12232495Pyridin-3-ylmethyl-hydrazineHCID 159380972-(2-Oxo-propyl)-benzo[D][1,3]oxazin-4-one

Produkt 1

HCID 22320205HCID 22320205, VerbindungAusbeute 67 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution in ethanol (50 mL) of 2-(2-oxopropyl)-4H-3,1-benzoxazin-4-one (11.2 g, 55.1 mmol) and 3-hydrazinomethylpyridine (7.44 g, 60.4 mmol) which was prepared from 3-chloromethylpyridine following the method described in Reference Example 2-2, was heated under reflux for 1 hour. The solution was cooled to room temperature, and the resulting crude crystals were collected by filtration. The crystals were washed with ethanol and air dried to give the title compound (11.3 g, 67% yield). mp: 180-183° C. (recrystallized from ethanol).

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hour
  3. filtrationthe resulting crude crystals were collected by filtration
  4. washThe crystals were washed with ethanol and air
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-cf44457fb6344e3fba6132667320dab9
Quelldatensatz
uspto-grants-2005_09
Patentnummer
US06949648B2

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