Methyl vinyl ketone → HCID 86734689, 화합물

HRID 329021

반응식

HRID 329021 반응식
[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

참가 물질

4

반응물 2

HCID 6570Methyl vinyl ketone2회HCID 86734686(+/-)-trans-1,2,3,4,4a,8,9,14a-Octahydropyrido[4',3':2,3]indolo[1,7-ab][1]benzazepine

생성물 1

HCID 86734689HCID 86734689, 화합물수율 86.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-26158a1e72fa4421acd3e10164e0b61a
출처 데이터셋
uspto-grants-1977_04
특허 번호
US04018930

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