Triethylamine → HCID 178471604, Verbindung

HRID 26128

Reaktionsgleichung

Reaktionsgleichung von HRID 26128
C(N(CC)CC)C.Cl.[NH2:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14].Cl[C:19]1[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2[S:21](=[O:29])(=[O:28])[N:20]=1>O1CCOCC1>[O:28]=[S:21]1(=[O:29])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=2[C:19]([NH:9][CH2:10][CH2:11][CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:20]1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 64783Pseudosaccharin chlorideHCID 126496614-Aminobutyrate ethyl hydrochloride

Produkt 1

HCID 178471604HCID 178471604, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

4.07 ml (29.2 mM) of triethylamine is added to 5.0 g. (29.2 mM) of ethyl 4-aminobutyrate hydrochloride, suspended in 75 ml of dioxane. After stirring for 5 minutes, 5.88 g. (29.2 mM) of 3-chloro-1,2-benzisothiazole 1,1-dioxide is added and the mixture is refluxed for one hour. The solvent is evaporated in vacuo and the residue is taken up in chloroform, washed with water, and evaporated to dryness. The residual 4-[(1,1-dioxo-1,2-benzisothiazol-3-yl)amino]-butanoic acid, ethyl ester is recrystallized from 40 ml. of methanol/water, yield 3.72 g., m.p. 125°-127°.

Aufarbeitung

  1. temperaturethe mixture is refluxed for one hour
  2. customThe solvent is evaporated in vacuo
  3. washwashed with water
  4. customevaporated to dryness
  5. customThe residual 4-[(1,1-dioxo-1,2-benzisothiazol-3-yl)amino]-butanoic acid, ethyl ester is recrystallized from 40 ml

Quellen und Nachweise

ORD-Eintrag
ord-2073cfa5dfc644b1b7a11fd14d15da28
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04148798

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