N-Ethoxymethanamine → HCID 14011488, Verbindung

HRID 246991Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 246991
[CH3:1][C:2]1([CH3:21])[CH2:6][C:5]2[CH:7]=[C:8]([O:11][C:12]3[CH:17]=[CH:16][C:15]([N:18]=[C:19]=[O:20])=[CH:14][CH:13]=3)[CH:9]=[CH:10][C:4]=2[O:3]1.[CH3:22][NH:23][O:24][CH2:25][CH3:26]>C1(C)C=CC=CC=1>[CH3:1][C:2]1([CH3:21])[CH2:6][C:5]2[CH:7]=[C:8]([O:11][C:12]3[CH:17]=[CH:16][C:15]([NH:18][C:19]([N:23]([O:24][CH2:25][CH3:26])[CH3:22])=[O:20])=[CH:14][CH:13]=3)[CH:9]=[CH:10][C:4]=2[O:3]1

Komponenten

4

Edukt 2

HCID 14895678N-EthoxymethanamineHCID 20161048HCID 20161048, Verbindung

Produkt 1

HCID 14011488HCID 14011488, VerbindungAusbeute 96,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

1.8 g of 4-(2,3-dihydro-2,2-dimethyl-5-benzofuranyloxy)phenyl isocyanate was dissolved in 20 ml of toluene, and 2.0 g of N-methyl-O-ethylhydroxylamine dissolved in 5 ml of toluene, was dropwise added thereto over a period of 20 minutes at room temperature. The mixture was stirred at room temperature for 2 hours, and then the solvent was distilled off. The residue was purified by silica gel column chromatography by using a solvent mixture of ethyl acetate/n-hexane=1/4 as the developer, to obtain 2.2 g of compound No. 29 as identified in Table 1.

Aufarbeitung

  1. additionwas dropwise added
  2. distillationthe solvent was distilled off
  3. customThe residue was purified by silica gel column chromatography
  4. additiona solvent mixture of ethyl acetate/n-hexane=1/4 as the developer

Quellen und Nachweise

ORD-Eintrag
ord-8f23056336404209a1e9e21294f6ca0a
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04705554

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