Methylamine → (S)-N-Methylhydroxysuccinimide

HRID 1981702

Reaktionsgleichung

Reaktionsgleichung von HRID 1981702
[C:1]([OH:9])(=O)[C@H:2]([CH2:4][C:5](O)=[O:6])[OH:3].[CH3:10][NH2:11]>C1(C)C=CC=CC=1>[OH:3][C@H:2]1[CH2:4][C:5](=[O:6])[N:11]([CH3:10])[C:1]1=[O:9]

Komponenten

4

Edukt 2

HCID 6329MethylamineHCID 222656L-Malic Acid

Produkt 1

HCID 13726417(S)-N-Methylhydroxysuccinimide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

To a stirred solution of 134 g (1 mole) of (S)-malic acid in 700 ml of toluene was added 97 ml of 40% aqueous methylamine. The temperature slowly rose to 50° C. After 0.5 hr the stirred mixture was heated to reflux and the water was collected in a Dean-Stark trap for 48 hr. A total of 93 ml of water was collected. The toluene residue was treated with 300 ml of ethanol and concentrated on the rotary evaporator. The residue was distilled. The yield of product obtained was 101 g (78%), b.p. 140°/2 mm; 145°/0.5 mm.

Aufarbeitung

  1. customslowly rose to 50° C
  2. temperatureAfter 0.5 hr the stirred mixture was heated
  3. temperatureto reflux
  4. customthe water was collected in a Dean-Stark trap for 48 hr
  5. customA total of 93 ml of water was collected
  6. additionThe toluene residue was treated with 300 ml of ethanol
  7. concentrationconcentrated on the rotary evaporator
  8. distillationThe residue was distilled
  9. customThe yield of product obtained
  10. custom145°/0.5 mm

Quellen und Nachweise

ORD-Eintrag
ord-4be2890a05fb4b93a178c10c47592717
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04592866

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