Sodium Hydroxide → (4-Methoxymethylbenzoylamino)-acetonitrile

HRID 568407

Reaktionsgleichung

Reaktionsgleichung von HRID 568407
[OH-].[Na+].S(=O)(=O)(O)O.[NH2:8][CH2:9][C:10]#[N:11].[CH3:12][O:13][CH2:14][C:15]1[CH:23]=[CH:22][C:18]([C:19](Cl)=[O:20])=[CH:17][CH:16]=1>O.C(OCC)(=O)C>[CH3:12][O:13][CH2:14][C:15]1[CH:23]=[CH:22][C:18]([C:19]([NH:11][CH2:10][C:9]#[N:8])=[O:20])=[CH:17][CH:16]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 196971Aminoacetonitrile sulfate (1:1)HCID 138793894-(Methoxymethyl)benzoyl chloride

Produkt 1

HCID 21273682(4-Methoxymethylbenzoylamino)-acetonitrile

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Sodium hydroxide (18.868, 0.47M) was dissolved in water (150 ml) and added to a stirred mixture of aminoacetonitrile bisulphate (24.23 g, 0.157M) and 4-methoxymethyl benzoyl chloride (29.9 g, 0.157M) in ethyl acetate (150 ml). The reaction was stirred for 21/2 hours at room temperature, the ethyl acetate layer was separated off and the aqueous layer re-extracted with ethyl acetate. The ethyl acetate extracts were combined, dried over magnesium sulphate and evaporated to give a white solid. This was recrystallised from chloroform 80:100 petrol to give white plates, (24.5 gm), mpt 107°-108° C.

Aufarbeitung

  1. customthe ethyl acetate layer was separated off
  2. extractionthe aqueous layer re-extracted with ethyl acetate
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customto give a white solid
  6. customThis was recrystallised from chloroform 80:100 petrol
  7. customto give white plates, (24.5 gm), mpt 107°-108° C.

Quellen und Nachweise

ORD-Eintrag
ord-8ce2c68f57a941858837c520a366fef0
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04728665

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