Triethylamine → Methyl 3-[2-[2-(5-methyl-2-thienyl)ethoxy]ethylaminosulphonyl]propanoate

HRID 1422277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1422277
[CH3:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH2:12])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl[S:21]([CH2:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])(=[O:23])=[O:22]>ClCCl>[CH3:1][C:2]1[S:6][C:5]([CH2:7][CH2:8][O:9][CH2:10][CH2:11][NH:12][S:21]([CH2:24][CH2:25][C:26]([O:28][CH3:29])=[O:27])(=[O:23])=[O:22])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 4962888Methyl 3-(chlorosulfonyl)propanoateHCID 195934942-[2-(5-Methyl-2-thienyl)ethoxy]ethanamine

Produkt 1

HCID 18779053Methyl 3-[2-[2-(5-methyl-2-thienyl)ethoxy]ethylaminosulphonyl]propanoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

The product of step c) as the hydrochloride salt (1.50 g) was stirred under nitrogen in dichloromethane (25 ml). Triethylamine (2.21 ml) was added followed by methyl 3-(chlorosulphonyl)propanoate (1.18 g). The mixture was stirred at room temperature overnight. The solution was diluted with a further amount of dichloromethane and the organics washed with dilute hydrochloric acid then water, then dried (MgSO4). The mixture was filtered and the volatiles removed in vacuo to give the subtitle compound as an oil (1.4 g).

Aufarbeitung

  1. washthe organics washed with dilute hydrochloric acid
  2. dry with materialwater, then dried (MgSO4)
  3. filtrationThe mixture was filtered
  4. customthe volatiles removed in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-85def47d92df43e882d58caea34ba83d
Quelldatensatz
uspto-grants-2000_06
Patentnummer
US06080869

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