Water → Diethyl 4-isothiocyanatobenzylphosphonate

HRID 25512

Reaktionsgleichung

Reaktionsgleichung von HRID 25512
[C:1](Cl)(Cl)=[S:2].[NH2:5][C:6]1[CH:20]=[CH:19][C:9]([CH2:10][P:11](=[O:18])([O:15][CH2:16][CH3:17])[O:12][CH2:13][CH3:14])=[CH:8][CH:7]=1.C(=O)(O)[O-].[Na+].O>ClCCl>[N:5]([C:6]1[CH:7]=[CH:8][C:9]([CH2:10][P:11](=[O:18])([O:12][CH2:13][CH3:14])[O:15][CH2:16][CH3:17])=[CH:19][CH:20]=1)=[C:1]=[S:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 10040ThiophosgeneHCID 88358Diethyl p-aminobenzylphosphonateHCID 516892Sodium Bicarbonate

Produkt 1

HCID 22568434Diethyl 4-isothiocyanatobenzylphosphonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Thiophosgene (4.1 mL, 54 mmol) was added al at once to a mixture of diethyl 4-aminobenzylphosphonate (12.04 g, 50 mmol), sodium bicarbonate (8.33 g, 99 mmol), water (100 mL), and dichloromethane (250 mL), and the mixture was stirred at room temperature for about 2 hours. The organic and aqueous layers were separated, the organic layer dried over magnesium sulfate, filtered, and concentrated to give the product isothiocyanate as a brown oil. This was used directly in the next step.

Aufarbeitung

  1. customThe organic and aqueous layers were separated
  2. dry with materialthe organic layer dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-2c8f5600ae6f41b9984d67f20d309d62
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06858739B2

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