Methylamine → HCID 13457740, Verbindung

HRID 462745Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 462745
[Cl:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[C:4]([C:6]1[N:7]([N:11]2C(=O)C3=CC=CC=C3C2=O)[CH:8]=[CH:9][CH:10]=1)=[O:5].CN>C(O)C.O>[NH2:11][N:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4](=[O:5])[C:3]1[CH:22]=[CH:23][CH:24]=[CH:25][C:2]=1[Cl:1]

Komponenten

5

Versuchsvorschrift

2-(2-chlorobenzoyl)-1-phthalimidopyrrole (40 g, 0.114 mmol) was suspended in 350 ml of 95% ethanol. To this rapidly stirred slurry was added 50 ml of a 40% aqueous solution of methylamine over 10 minutes. After 2.5 hours of rapid stirring the mixture was diluted with 400 ml of water and extracted with four 200 ml portions of ether. The combined extracts were washed with water, dried over anhydrous MgSO4, filtered and evaporated to an oil which solidified upon standing. Trituration of this solid with hexane and collection upon a filter yielded 23.6 g (94%) of solid, m.p. 76°-78°.

Aufarbeitung

  1. extractionextracted with four 200 ml portions of ether
  2. washThe combined extracts were washed with water
  3. dry with materialdried over anhydrous MgSO4
  4. filtrationfiltered
  5. customevaporated to an oil which
  6. customTrituration of this solid with hexane and collection upon a filter

Quellen und Nachweise

ORD-Eintrag
ord-61f8f72c70b741d8a97da55f6082dad7
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04517195

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