Ammonium thiocyanate → 1-isopropyl-4-phenyl-6,7-methylenedioxy-3,4-dihydro-2(1H)-quinazolinthione

HRID 1576517Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1576517
[CH:1]([NH:4][C:5]1[CH:18]=[C:17]2[O:19][CH2:20][O:21][C:16]2=[CH:15][C:6]=1[CH:7](O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:3])[CH3:2].[S-:22][C:23]#[N:24].[NH4+]>C(O)(=O)C>[CH:1]([N:4]1[C:5]2[C:6](=[CH:15][C:16]3[O:21][CH2:20][O:19][C:17]=3[CH:18]=2)[CH:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[NH:24][C:23]1=[S:22])([CH3:3])[CH3:2]

Komponenten

4

Edukt 2

HCID 15666Ammonium thiocyanateHCID 215113612-Isopropylamino-4,5-methylenedioxybenzhydrol

Produkt 1

HCID 127894811-isopropyl-4-phenyl-6,7-methylenedioxy-3,4-dihydro-2(1H)-quinazolinthione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To a solution of 1 gram of 2-isopropylamino-4,5-methylenedioxybenzhydrol and 28 mls. glacial acetic acid is added 2 grams of ammonium thiocyanate. The resultant mixture is stirred at room temperature for 24 hours to solid precipitates and is removed by filtration. The filtrate is evaporated to dryness and the residual solid taken up in chloroform. This solution is washed with water, dried and evaporated to dryness. The resulting solid is recrystallized from ethyl acetate to yield 1-isopropyl-4-phenyl-6,7-methylenedioxy-3,4-dihydro-2[1H]-quinazolinthione m.p. 214°-218°C.

Aufarbeitung

  1. customprecipitates
  2. customis removed by filtration
  3. customThe filtrate is evaporated to dryness
  4. washThis solution is washed with water
  5. customdried
  6. customevaporated to dryness
  7. customThe resulting solid is recrystallized from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-9d640453bbae42b787e3872951db5d38
Quelldatensatz
uspto-grants-1976_09
Patentnummer
US03981890

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