Hydrochloric Acid → 2-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride

HRID 622423Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 622423
P(=[S:5])([O-])([O-])[O-].[Na+].[Na+].[Na+].Cl.[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][Cl:19])[CH2:13]1.Cl>O>[ClH:19].[OH:10][N:11]=[C:12]1[CH2:16][CH2:15][N:14]([C:17](=[NH:20])[CH2:18][SH:5])[CH2:13]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 9877537Trisodium thiophosphateHCID 867424302-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride

Produkt 1

HCID 867424332-(3-Hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochlorideAusbeute 64,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

945 mg of trisodium phosphorothioate were added to a solution of 1.05 g of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylchloride hydrochloride in 6.4 ml of water, cooled with ice-water, and the mixture was stirred at room temperature for about one hour. 5.2 ml of 1N hydrochloric acid were added, and the mixture was heated at 65° C. for 30 minutes and then concentrated under reduced pressure. The concentrate was mixed with 5.2 ml of methanol, insolubles were filtered off, and the filtrate was concentrated under reduced pressure. Anhydrous ether was added to the concentrate, and the precipitated crystals were collected by filtration and washed with ether, giving 670 mg of 2-(3-hydroxyiminopyrrolidin-1-yl)-2-iminoethylmercaptan hydrochloride.

Aufarbeitung

  1. temperaturethe mixture was heated at 65° C. for 30 minutes
  2. concentrationconcentrated under reduced pressure
  3. additionThe concentrate was mixed with 5.2 ml of methanol, insolubles
  4. filtrationwere filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. additionAnhydrous ether was added to the concentrate
  7. filtrationthe precipitated crystals were collected by filtration
  8. washwashed with ether

Quellen und Nachweise

ORD-Eintrag
ord-02014e8f7cfa476889b69de7191d4aee
Quelldatensatz
uspto-grants-1988_09
Patentnummer
US04771046

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