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

HRID 1576517ノート

反応式

HRID 1576517 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9d640453bbae42b787e3872951db5d38
出典データセット
uspto-grants-1976_09
特許番号
US03981890

反応ノート

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