Hydrochloric Acid → HCID 57673909, Verbindung

HRID 490058Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 490058
[NH2:1][C:2]([CH2:25][OH:26])([CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:13][CH:12]=1)[CH2:3][O:4][P:5](=[O:8])([OH:7])[OH:6].C(N([CH2:43][C:44]([OH:46])=O)CC(O)=O)CN(CC(O)=O)CC(O)=O.B(O)(O)O.Cl>C(O)C>[OH:26][CH2:25][C:2]([N:1]1[CH2:12][C:11]2[C:43](=[CH:3][CH:2]=[CH:9][CH:10]=2)[C:44]1=[O:46])([CH2:9][CH2:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:15][CH:16]=1)[CH2:3][O:4][P:5](=[O:6])([OH:7])[OH:8]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 6049Ethylenediaminetetraacetic AcidHCID 7628Boric AcidHCID 9908268Fingolimod phosphate

Produkt 1

HCID 57673909HCID 57673909, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

The endproduct of step d) ((R/S)-FTY720-phosphate) (50 mg; 0.125 mmol) is suspended in a solution of EDTA (0.5 ml; 10 mM in water) and aqueous boric acid (0.5 ml; 3% in water; adjusted to pH 10.5 with aqueous KOH10%). After addition of OPA (33 mg, 0.25 mmol), dissolved in ethanol (0.5 ml), the reaction is kept at RT for 1 hour (ultrasound). After that the pH is adjusted to 3.5 (aqueous HCl; 1N) and extracted with ethylacetate (three times). The organic layer is dried over Na2SO4 and the compound is purified on silica gel using methylenechloride/methanol (95/5→0/100) as mobile phase.

Aufarbeitung

  1. additionAfter addition of OPA (33 mg, 0.25 mmol)
  2. extractionextracted with ethylacetate (three times)
  3. dry with materialThe organic layer is dried over Na2SO4
  4. customthe compound is purified on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-3686e9d92cd049048910744240f2e15e
Quelldatensatz
uspto-grants-2009_05
Patentnummer
US07528120B2

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