4-Methylmorpholine → HCID 71623011, Verbindung

HRID 1477510Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1477510
[NH2:1][C:2]([CH3:6])([CH3:5])[C:3]#[N:4].CN1CC[O:11][CH2:10][CH2:9]1.O1C=[C:17]([C:19](Cl)=[O:20])[N:16]=[N:15]1>ClCCl>[C:3]([C:2]([NH:1][C:19]([C:17]1[O:11][C:10]([CH3:9])=[N:15][N:16]=1)=[O:20])([CH3:6])[CH3:5])#[N:4]

Komponenten

5

Versuchsvorschrift

2-Amino-2-methylpropanenitrile (90 gms) was suspended in dichloromethane (90 ml) and N-methyl morpholine (1.10 moles) was added with stirring. A mixture of oxadiazole carbonyl chloride (90 gms) in dichloromethane (100 ml) was added drop wise to the suspension at 0 to 5° C. The reaction mixture was stirred and monitored by thin layer chromatography (TLC). The reaction mass was concentrated under reduced pressure after completion of reaction. The product separated out on addition of isopropyl alcohol (500 ml), which was then filtered and dried.

Aufarbeitung

  1. additionwas added drop wise to the suspension at 0 to 5° C
  2. stirringThe reaction mixture was stirred
  3. concentrationThe reaction mass was concentrated under reduced pressure
  4. customafter completion of reaction
  5. customThe product separated out on addition of isopropyl alcohol (500 ml), which
  6. filtrationwas then filtered
  7. customdried

Quellen und Nachweise

ORD-Eintrag
ord-0732dca887ce45029ae35522cc088920
Quelldatensatz
uspto-grants-2016_08
Patentnummer
US09403809B2

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