Methanesulfonyl isocyanate → HCID 13768039, Verbindung

HRID 1789354Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1789354
[F:1][C:2]1[CH:3]=[C:4]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][O:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[CH:23]3[NH:27][CH2:26][CH2:25][S:24]3)[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.[CH3:28][S:29]([N:32]=[C:33]=[O:34])(=[O:31])=[O:30]>CC(C)=O>[CH3:28][S:29]([NH:32][C:33]([N:27]1[CH2:26][CH2:25][S:24][CH:23]1[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[O:16][CH2:15][CH2:14][N:11]1[CH2:12][CH2:13][N:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([F:1])[CH:3]=2)[CH2:9][CH2:10]1)=[O:34])(=[O:31])=[O:30]

Komponenten

4

Edukt 2

HCID 12668338Methanesulfonyl isocyanateHCID 13768101HCID 13768101, Verbindung

Produkt 1

HCID 13768039HCID 13768039, VerbindungAusbeute 61,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

1.94 g of 2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazolidine are dissolved in anhydrous acetone, and 0.73 g of methanesulfonyl isocyanate is added thereto at room temperature. After the mixture is stirred for 30 minutes, the mixture is concentrated under reduced pressure to remove solvent. The residue is collected by filtration, and washed with water and ether, successively. The crude product thus obtained is recrystallized from a mixture of acetone and ether. 1.56 g of N-methanesulfonyl-2-{2-[2-(4-(3-fluorophenyl)piperazin-1-yl)ethyloxy]phenyl}thiazollidine-3-carboxamide are obtained.

Aufarbeitung

  1. customat room temperature
  2. concentrationthe mixture is concentrated under reduced pressure
  3. customto remove solvent
  4. filtrationThe residue is collected by filtration
  5. washwashed with water and ether
  6. customThe crude product thus obtained
  7. customis recrystallized from a mixture of acetone and ether

Quellen und Nachweise

ORD-Eintrag
ord-4309e47a359d4d8aa7980c2c2a42a140
Quelldatensatz
uspto-grants-1987_08
Patentnummer
US04689327

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