Methanesulfonyl chloride → Methyl 5-methanesulfonylamino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

HRID 2269800Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2269800
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:12]2[C:17]([O:18][CH2:19][O:20][CH3:21])=[CH:16][CH:15]=[CH:14][C:13]=2[O:22][CH3:23])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].[CH3:24][S:25](Cl)(=[O:27])=[O:26]>N1C=CC=CC=1>[CH3:24][S:25]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([C:12]2[C:17]([O:18][CH2:19][O:20][CH3:21])=[CH:16][CH:15]=[CH:14][C:13]=2[O:22][CH3:23])=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8])(=[O:27])=[O:26]

Komponenten

4

Edukt 2

HCID 31297Methanesulfonyl chlorideHCID 18188782Methyl 5-amino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

Produkt 1

HCID 18189252Methyl 5-methanesulfonylamino-2-(2-methoxy-6-methoxymethoxyphenyl)-benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A solution of Example 32B (10 g, 34.8 mmol), in pyridine (50 mL) at room temperature was treated with methanesulfonyl chloride (2.7 mL, 34.8 mmol), stirred at room temperature for 16 hours, and concentrated. The concentrate was treated with ethyl acetate (100 mL), and the resulting solution was washed with 2N HCl, dried (Na2SO4), filtered, and concentrated. The concentrate was recrystallized from ethanol to provide the desired product. MS (ESI(−)Q1MS) m/z 394 (M−H)−.

Aufarbeitung

  1. concentrationconcentrated
  2. additionThe concentrate was treated with ethyl acetate (100 mL)
  3. washthe resulting solution was washed with 2N HCl
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-297a8da4f83d47e68200283e16c6310b
Quelldatensatz
uspto-grants-2001_12
Patentnummer
US06329534B1

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