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

HRID 1576517노트

반응식

HRID 1576517 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d640453bbae42b787e3872951db5d38
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03981890

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