Phosphoric Acid → HCID 58972470, Verbindung

HRID 30993Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 30993
[CH3:1][O:2][C:3](=[O:29])[CH2:4][N:5]1[C:11](=[O:12])[C@@H:10]([NH:13]C(OC(C)(C)C)=O)[C:9]2[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=2[C:7]2[CH:25]=[CH:26][CH:27]=[CH:28][C:6]1=2.P(=O)(O)(O)O.[OH-].[Na+]>ClCCl>[CH3:1][O:2][C:3](=[O:29])[CH2:4][N:5]1[C:11](=[O:12])[C@@H:10]([NH2:13])[C:9]2[CH:21]=[CH:22][CH:23]=[CH:24][C:8]=2[C:7]2[CH:25]=[CH:26][CH:27]=[CH:28][C:6]1=2

Komponenten

5

Edukt 3

HCID 1004Phosphoric AcidHCID 14798Sodium HydroxideHCID 58972533((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester

Produkt 1

HCID 58972470HCID 58972470, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

((S)-7-tert-Butoxycarbonylamino-6-oxo-6,7-dihydro-dibenzo[b,d]azepin-5-yl)-acetic acid methyl ester (60 mg, 0.15 mmol) were dissolved in dichloromethane (3 ml), treated with 0.15 ml (2.3 mmol) orthophosphoric acid and stirred for 18 .h The reaction mixture is adjusted to pH 7.5 with 2N aqueous sodium hydroxide, diluted with dichloromethane (5 ml) and the phases separated. After extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml), the solution is dried with magnesium sulfate and evaporated to dryness. White solid (60%); MS: m/e=297(M+H+), which was used without further purification.

Aufarbeitung

  1. customthe phases separated
  2. extractionAfter extraction of the organic phases with water (5 ml) and saturated aqueous sodium chloride (5 ml)
  3. dry with materialthe solution is dried with magnesium sulfate
  4. customevaporated to dryness
  5. customMS: m/e=297(M+H+), which was used without further purification

Quellen und Nachweise

ORD-Eintrag
ord-50155863f6ec4ac090cace69e4b37baf
Quelldatensatz
uspto-grants-2008_09
Patentnummer
US07425551B2

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