Triethylamine → HCID 68881182, Verbindung

HRID 915904Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 915904
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:15](O)[CH2:16][N+:17]([O-:19])=[O:18])[CH:6]=[CH:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1.C(N(CC)CC)C.CS(Cl)(=O)=O>ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5](/[CH:15]=[CH:16]\[N+:17]([O-:19])=[O:18])[CH:6]=[CH:7][C:8]=1[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 68880923HCID 68880923, Verbindung

Produkt 1

HCID 68881182HCID 68881182, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 1-(3-methoxy4-pyridin-2-ylphenyl)-2-nitroethanol (290 mg, 1.06 mmol) in anhydrous dichloromethane (5 mL) was treated with triethylamine (0.24 mL, 1.69 mmol), followed by methanesulfonyl chloride (0.10 mL, 1.27 mmol), 1 hr later, the mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL). The phases were separated and the aqueous layer was extracted with dichloromethane (3×10 mL). The combined organic layers were dried (MgSO4), filtered and concentrated to afford a yellow solid.

Aufarbeitung

  1. customthe mixture was partitioned between sat. NaHCO3 (10 mL) and dichloromethane (20 mL)
  2. customThe phases were separated
  3. extractionthe aqueous layer was extracted with dichloromethane (3×10 mL)
  4. dry with materialThe combined organic layers were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto afford a yellow solid

Quellen und Nachweise

ORD-Eintrag
ord-7786f7818b24484b96c2d24998eac6d3
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07268151B2

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