Water → HCID 86752944, Verbindung

HRID 1957579Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1957579
C[O:2][C:3](=[O:39])[C@@H:4]([NH:31][S:32]([CH2:35][CH2:36][CH2:37][CH3:38])(=[O:34])=[O:33])[CH2:5][NH:6][C:7]([C:9]1[O:13][N:12]=[C:11]([O:14][CH2:15][CH2:16][CH2:17][CH:18]2[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]2)[CH:10]=1)=[O:8].O[Li].O.O.OS([O-])(=O)=O.[Na+]>C1COCC1>[C:24]([N:21]1[CH2:20][CH2:19][CH:18]([CH2:17][CH2:16][CH2:15][O:14][C:11]2[CH:10]=[C:9]([C:7]([NH:6][CH2:5][C@H:4]([NH:31][S:32]([CH2:35][CH2:36][CH2:37][CH3:38])(=[O:34])=[O:33])[C:3]([OH:39])=[O:2])=[O:8])[O:13][N:12]=2)[CH2:23][CH2:22]1)([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25]

Komponenten

6

Edukt 4

HCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 516919Sodium BisulfateHCID 86752943HCID 86752943, Verbindung

Produkt 1

HCID 86752944HCID 86752944, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 3-8 (1.86 mg, 0.32 mmol), LiOH.H2O (67 mg, 1.6 mmol), H2O (2 mL), and THF (8 mL) was stirred at ambient temperature for 1.0 h. The solution was acidified with 1M NaHSO4 followed by evaporation of THF. The residue was partitioned between EtOAc and brine. The EtOAc layer was then dried (MgSO4) and concentrated to give 3-9 as a pale yellow solid. Rf 0.40 (silica, 9/.0.5/0.5 CH2Cl2 :CH3OH:HOAc).

Aufarbeitung

  1. customfollowed by evaporation of THF
  2. customThe residue was partitioned between EtOAc and brine
  3. dry with materialThe EtOAc layer was then dried (MgSO4)
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-64da6f58d0bf45ea8ee01a8bf3c0e615
Quelldatensatz
uspto-grants-1998_07
Patentnummer
US05786373

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