Triethylamine → 3-methyl-4-(methanesulfonamido)phenyl N-methylcarbamate

HRID 2072422Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2072422
[CH3:1][NH:2][C:3](=[O:13])[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[C:7]([CH3:12])[CH:6]=1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23]>C1C=CC=CC=1>[CH3:1][NH:2][C:3](=[O:13])[O:4][C:5]1[CH:10]=[CH:9][C:8]([NH:11][S:22]([CH3:21])(=[O:24])=[O:23])=[C:7]([CH3:12])[CH:6]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 25072AminomatacilHCID 31297Methanesulfonyl chloride

Produkt 1

HCID 214093123-methyl-4-(methanesulfonamido)phenyl N-methylcarbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 241BenzeneLösungsmittel

Versuchsvorschrift

A flask was charged with 3-methyl-4-aminophenyl N-methylcarbamate (3.0g., 0.0166 mole), triethylamine (1.83g., 0.018 mole, 2.53 ml.) and about 100 ml. of benzene. To this slurry was added methanesulfonyl chloride and after one hour at reflux the mixture was cooled and filtered. The solids were stirred vigorously with water to dissolve any residual by-product triethylamine hydrochloride. Refiltration and drying gave 2.3g. of the desired product (m.p. 167°-69° C.).

Aufarbeitung

  1. temperatureafter one hour at reflux the mixture
  2. temperaturewas cooled
  3. filtrationfiltered
  4. dissolutionto dissolve any residual by-product triethylamine hydrochloride
  5. customRefiltration and drying
  6. customgave 2.3g

Quellen und Nachweise

ORD-Eintrag
ord-24181135411a42c3a879bb8b177c34a6
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04051254

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