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

HRID 1973437ノート

反応式

HRID 1973437 の反応式
[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]

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-74718446bf124ff6957b36c0dc1ec4a0
出典データセット
uspto-grants-1976_12
特許番号
US03997564

反応ノート

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