Diisopropylethylamine → 1-(2,3-Dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide

HRID 482960Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 482960
[CH3:1][O:2][N:3]([CH3:7])[C:4](Cl)=[O:5].[NH:8]([C:10]1[C:18]2[O:17][CH:16]([CH3:19])[CH2:15][C:14]=2[CH:13]=[CH:12][CH:11]=1)[NH2:9].C(N(C(C)C)CC)(C)C>C1COCC1>[CH3:19][CH:16]1[CH2:15][C:14]2[CH:13]=[CH:12][CH:11]=[C:10]([NH:8][NH:9][C:4]([N:3]([O:2][CH3:1])[CH3:7])=[O:5])[C:18]=2[O:17]1

Komponenten

5

Edukt 3

HCID 81531DiisopropylethylamineHCID 2734926N-methoxy-N-methylcarbamoyl chlorideHCID 135358277-Hydrazino-2,3dihydro-2-methylbenzofuran

Produkt 1

HCID 135358281-(2,3-Dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

4.9 g of N-methoxy-N-methylcarbamic chloride was added drop-by-drop (over 5 minutes) to a mixture of 6.6 g of 1D, 125 ml of THF and 5.2 g of N,N-diisopropyl-N-ethylamine, at -10° C. The mixture was stirred for 1 hour at 0° C., and then mixed with ice water. The resulting mixture was extracted with ether, the extract was dried (MgSO4) and the solvent was evaporated, to give 1-(2,3-dihydro-2-methylbenzofuran-7-yl)-4-methoxy-4-methylsemicarbazide (1E), as an amber syrup.

Aufarbeitung

  1. extractionThe resulting mixture was extracted with ether
  2. dry with materialthe extract was dried (MgSO4)
  3. customthe solvent was evaporated

Quellen und Nachweise

ORD-Eintrag
ord-f49ff24e0d824e47998caab9fdd77aea
Quelldatensatz
uspto-grants-1986_03
Patentnummer
US04577011

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