Dichloromethane → HCID 14476476, Verbindung

HRID 1492164Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1492164
[C:1]([NH:4][C:5]1[CH:6]=[C:7]([CH:9]=[CH:10][CH:11]=1)[NH2:8])(=[O:3])[CH3:2].ClCCl.[CH3:15][C:16]([CH3:21])=[CH:17][C:18](Cl)=[O:19]>C(N(CC)CC)C>[C:1]([NH:4][C:5]1[CH:11]=[CH:10][CH:9]=[C:7]([NH:8][C:18](=[O:19])[CH:17]=[C:16]([CH3:21])[CH3:15])[CH:6]=1)(=[O:3])[CH3:2]

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 7604m-AminoacetanilideHCID 1023943-Methyl-2-butenoyl chloride

Produkt 1

HCID 14476476HCID 14476476, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

56.7 g. ( 0.42 mole ) 3-acetamidoaniline in 400 ml. dichloromethane and 65 ml. ( 0.46 tool ) triethylamine are mixed, while cooling with ice, with 59.0 g. (0.46 mole) 3,3-dimethylacryloyl chloride and stirred for 2 hours at ambient temperature. The solution is thereafter extracted with water and the separated organic phase is dried over anhydrous sodium sulphate, evaporated and the residue mixed with ethyl acetate. Upon standing in a refrigerator, crystals separate out. Yield 45.7 g. (47% of theory); m.p. 144°-148° C.

Aufarbeitung

  1. temperaturewhile cooling with ice, with 59.0 g
  2. extractionThe solution is thereafter extracted with water
  3. dry with materialthe separated organic phase is dried over anhydrous sodium sulphate
  4. customevaporated
  5. additionthe residue mixed with ethyl acetate
  6. customseparate out

Quellen und Nachweise

ORD-Eintrag
ord-63ae773b3cb74f3e97e5d7dbf6a30399
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05373019

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