Methyl vinyl ketone → HCID 86734689、化合物

HRID 329021

反応式

HRID 329021 の反応式
[CH:1]([C:3]([CH3:5])=[O:4])=[CH2:2].[CH2:6]1[C@@H:16]2[C@H:10]([CH:11]=[CH:12][C:13]3[C:14]4[N:15]2[C:17]2[CH:26]=[CH:25][N:24]=[CH:23][C:18]=2[C:19]=4[CH2:20][CH2:21][CH:22]=3)[CH2:9][CH2:8][CH2:7]1>C(O)C>[CH2:6]1[CH:16]2[CH:10]([CH:11]=[CH:12][C:13]3[C:14]4[N:15]2[C:17]2[CH:26]=[CH:25][N:24]=[CH:23][C:18]=2[C:19]=4[CH2:20][CH2:21][CH:22]=3)[CH2:9][CH:8]([CH2:2][CH2:1][C:3](=[O:4])[CH3:5])[CH2:7]1

参加物

4

反応物 2

HCID 6570Methyl vinyl ketone2 回HCID 86734686(+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

生成物 1

HCID 86734689HCID 86734689、化合物収率 86.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.3 grams of methyl vinyl ketone was added to a solution of 8.3 grams of (±)-trans-1,2,3,4,4a,8,9,14a-octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine in 400 ml. of ethanol. The mixture was permitted to stand at room temperature for four days, after which an additional 2.6 grams of methyl vinyl ketone was added. This mixture was permitted to stand at room temperature for three days, and was then filtered, evaporated to dryness in vacuo, and triturated with pentane. The resulting solid was recrystallized from ethanol to yield 9 grams of the title compound with m.p. 102.5° C.

後処理

  1. waitto stand at room temperature for three days
  2. filtrationwas then filtered
  3. customevaporated to dryness in vacuo
  4. customtriturated with pentane
  5. customThe resulting solid was recrystallized from ethanol

出典と根拠

ORDレコード
ord-26158a1e72fa4421acd3e10164e0b61a
出典データセット
uspto-grants-1977_04
特許番号
US04018930

関連ノート

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