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

HRID 1973437노트

반응식

HRID 1973437 반응식
[CH:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]3[O:16][CH2:15][O:14][C:11]=3[CH:12]=2)[CH:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[NH:6][C:5]1=[S:23])([CH3:3])[CH3:2]>[O-2].[O-2].[Mn+4].C(Cl)Cl>[CH:1]([N:4]1[C:13]2[C:8](=[CH:9][C:10]3[O:16][CH2:15][O:14][C:11]=3[CH:12]=2)[C:7]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[N:6][C:5]1=[S:23])([CH3:3])[CH3:2]

참가 물질

4

반응물 1

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

생성물 1

HCID 127894951-isopropyl-4-phenyl-6,7-methylenedioxy-2(1H)-quinazolinthione

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 6344Dichloromethane용매

실험 절차

A mixture of 2 grams of 1-isopropyl-4-phenyl-6,7-methylenedioxy-3,4-dihydro-2(1H)-quinazolinthione, 100 ml. of methylene chloride and 4 grams of manganese dioxide is stirred for 48 hours at room temperature. Precipitated solids are removed by filtration and the filtrate evaporated to dryness. The residue is recrystallized from ethyl acetate and then methanol and then eluted with benzene in a silica gel column to give 1-isopropyl-4-phenyl-6,7-methylenedioxy-2(1H)-quinazolinthione, m.p. 202°-205°C.

후처리

  1. customPrecipitated solids
  2. customare removed by filtration
  3. customthe filtrate evaporated to dryness
  4. customThe residue is recrystallized from ethyl acetate
  5. washmethanol and then eluted with benzene in a silica gel column

출처 및 근거

ORD 기록
ord-74718446bf124ff6957b36c0dc1ec4a0
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03997564

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