Dichloromethane → HCID 57378117, Verbindung

HRID 511907

Reaktionsgleichung

Reaktionsgleichung von HRID 511907
C(N(CC)CC)C.[C:8]([N:15]1[CH:19]=[CH:18]N=C1)(N1C=CN=C1)=[S:9].C(Cl)Cl.NC1C=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1>C(OCC)(=O)C>[N:15]([C:19]1[CH:18]=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1)=[C:8]=[S:9]

Komponenten

6

Edukt 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 802641,1'-ThiocarbonyldiimidazoleHCID 2357134-Amino-2-nitrobenzoic Acid

Produkt 1

HCID 57378117HCID 57378117, VerbindungAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

Triethylamine (55.8 μL, 0.4 mmol) and thiocarbonyldiimidazole (46.3 mg, 0.26 mmol) were added to a methylene chloride solution (0.4 mL) of 4-amino-2-nitrobenzoic acid (36.4 mg, 0.2 mmol) at room temperature, followed by stirring at room temperature for 10 minutes. The reaction mixture was dissolved in ethyl acetate and washed with 1 M hydrochloric acid, the organic layer was separated, and then the organic layer was dried over magnesium sulfate. Thereafter, filtration and concentration under reduced pressure to dryness were carried out to obtain 4-isothiocyanato-2-nitrobenzoic acid as a colorless solid (40 mg, yield: 89%, HPLC purity: 96.4%)

Aufarbeitung

  1. washwashed with 1 M hydrochloric acid
  2. customthe organic layer was separated
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. filtrationThereafter, filtration and concentration under reduced pressure to dryness

Quellen und Nachweise

ORD-Eintrag
ord-3ec28024c9bd4081b8104eea24de2c4b
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09102602B2

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