Chloroacetyl chloride → Chloroacetic acid morpholine carboxamide

HRID 1418007

Reaktionsgleichung

Reaktionsgleichung von HRID 1418007
[Cl:1][CH2:2][C:3](Cl)=[O:4].C[N:7]1CC[O:10]CC1.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>ClCCl>[N:13]1([C:3]([NH2:7])=[O:4])[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.[Cl:1][CH2:2][C:3]([OH:4])=[O:10]

Komponenten

5

Versuchsvorschrift

Combine chloroacetyl chloride (2.00 mL, 25.0 mmol) and N-methylmorpholine (2.76 mL, 25.0 mmol) in dichloromethane (100 mL). Cool in an ice-bath. Add morpholine (2.19 mL, 25.0 mmol) and stir in the ice-bath for 1 hour. Warm to ambient temperature and stir for 1 hour. Extract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to obtain chloroacetic acid morpholine carboxamide.

Aufarbeitung

  1. temperatureCool in an ice-bath
  2. extractionExtract with cold aqueous 5% sulfuric acid solution, saturated aqueous sodium bicarbonate solution, and saturated aqueous sodium chloride solution
  3. dry with materialDry the organic layer over Na2SO4
  4. filtrationfilter
  5. customevaporate in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-574c4b28fe3449deb3cc7d1c2a44718a
Quelldatensatz
uspto-grants-1999_03
Patentnummer
US05880119

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