Phosphorus trichloride → HCID 11217864, Verbindung

HRID 1421637Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1421637
P(Cl)(Cl)Cl.[CH2:5]([NH:11][C@H:12]([C:17]([OH:19])=[O:18])[CH2:13][C:14]([OH:16])=O)[CH2:6][C:7]([CH3:10])([CH3:9])[CH3:8]>C(O)(=O)C>[CH2:5]([NH:11][C@@H:12]1[C:17](=[O:18])[O:19][C:14](=[O:16])[CH2:13]1)[CH2:6][C:7]([CH3:8])([CH3:9])[CH3:10]

Komponenten

4

Edukt 2

HCID 24387Phosphorus trichlorideHCID 9815811N-(3,3-Dimethylbutyl)-L-aspartic acid

Produkt 1

HCID 11217864HCID 11217864, VerbindungAusbeute 69,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Phosphorous trichloride (3.7 ml, 43 mmol) was added, dropwise, to a 10° C. slurry of N-neohexyl-L-aspartic acid (11.6 g, 53.4 mmol) in glacial acetic acid (50 ml). After addition was complete (0.5 hr), the resulting clear solution was stirred at room temperature overnight. The resulting solid precipitate was collected by vacuum filtration, washed with acetic acid and methylene chloride, then dried at 35-40° C. for 3 hours to give 3.62 g (69.8%) of pure N-neohexyl-L-aspartic anhydride.

Aufarbeitung

  1. customto a 10° C.
  2. additionAfter addition
  3. custom(0.5 hr)
  4. filtrationThe resulting solid precipitate was collected by vacuum filtration
  5. washwashed with acetic acid and methylene chloride
  6. customdried at 35-40° C. for 3 hours

Quellen und Nachweise

ORD-Eintrag
ord-15f9213427d048fb84acc86359840fb7
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06077962

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