Water → 2,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamate

HRID 435805

Reaktionsgleichung

Reaktionsgleichung von HRID 435805
[CH3:1][C:2]1([CH3:16])[O:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[O:11][C:12]([NH:14][CH3:15])=[O:13])[CH2:3]1.[O:17]1[CH2:22][CH2:21][N:20]([S:23]Cl)[CH2:19][CH2:18]1.Cl.N1C=CC=CC=1.O>N1C=CC=CC=1>[CH3:15][N:14]([S:23][N:20]1[CH2:21][CH2:22][O:17][CH2:18][CH2:19]1)[C:12](=[O:13])[O:11][C:8]1[C:9]2[O:10][C:2]([CH3:16])([CH3:1])[CH2:3][C:4]=2[CH:5]=[CH:6][CH:7]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 2566CarbofuranHCID 10176127Pyridinium chlorideHCID 122977794-Morpholinesulfenyl chloride

Produkt 1

HCID 413832,3-Dihydro-2,2-dimethyl-7-benzofuranyl methyl(4-morpholinylthio)carbamateAusbeute 60,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

A mixture of 6.6 g of carbofuran and 4.8 g of morpholinosulfenyl chloride in 40 ml of pyridine was allowed to stand at room temperature for about 18 hours. The mixture, which contained solid pyridine hydrochloride, was poured into water and the aqueous mixture extracted with diethyl ether. The ether extract was washed with dilute acid, then with water and with saturated sodium chloride solution and dried. Evaporation of the ether gave 6.1 g of 2,3-dihydro-2,2-dimethyl-7-benzofuranyl (methyl)(morpholinosulfenyl)carbamate, m.p. 75° -78° . Recrystallization from hexane-diethyl ether increased the melting point to 89° .

Aufarbeitung

  1. extractionthe aqueous mixture extracted with diethyl ether
  2. extractionThe ether extract
  3. washwas washed
  4. additionwith dilute acid
  5. dry with materialwith water and with saturated sodium chloride solution and dried
  6. customEvaporation of the ether

Quellen und Nachweise

ORD-Eintrag
ord-68289026b5b44592bd76e0767cbb162a
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04006231

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