Lithium Hydroxide → 4-(2-Carboxymethoxy-ethylamino)-3-nitro-benzoic acid

HRID 1629828

Reaktionsgleichung

Reaktionsgleichung von HRID 1629828
[N:1]1([C:8]2[CH:17]=[CH:16][C:11]([C:12]([O:14]C)=[O:13])=[CH:10][C:9]=2[N+:18]([O-:20])=[O:19])[CH2:6][CH2:5][O:4][CH2:3][C:2]1=[O:7].[OH-:21].[Li+]>CO>[C:2]([CH2:3][O:4][CH2:5][CH2:6][NH:1][C:8]1[CH:17]=[CH:16][C:11]([C:12]([OH:14])=[O:13])=[CH:10][C:9]=1[N+:18]([O-:20])=[O:19])([OH:21])=[O:7]

Komponenten

4

Versuchsvorschrift

400 mg (1.43 mmol) methyl 4-(morpholin-3-on-4-yl)-3-nitro-benzoate are dissolved in 15 ml of methanol and combined with 4.5 ml (4.5 mmol) 1-molar lithium hydroxide solution. The mixture is stirred for 2 hours at ambient temperature. Then it is evaporated down i. vac., the residue is diluted with water, cooled in the ice bath and acidified with 2-molar hydrochloric acid. After 10 minutes cooling in the ice bath the precipitate formed is filtered off, washed with water until neutral and dried at 50° C. in the drying cupboard.

Aufarbeitung

  1. customThen it is evaporated down i
  2. addition, the residue is diluted with water
  3. temperaturecooled in the ice bath
  4. temperatureAfter 10 minutes cooling in the ice bath the precipitate
  5. customformed
  6. filtrationis filtered off
  7. washwashed with water until neutral and
  8. customdried at 50° C. in the drying cupboard

Quellen und Nachweise

ORD-Eintrag
ord-9179d167fff44d47b90f3534a8d7ceab
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08791103B2

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