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HCID 57092295, 화합물 → HCID 53975106, 화합물

HRID 1031031
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HRID 1031031 반응식
[CH:1]([C:4]([CH3:22])([N:7]1[C:11](=[O:12])[CH:10]2[CH2:13][CH2:14][C:15]3[N:16]([CH3:20])[CH:17]=[CH:18][C:19]=3[CH:9]2[C:8]1=[O:21])[C:5]#[N:6])([CH3:3])[CH3:2]>ClC1C=CC=CC=1.[O-2].[O-2].[Mn+4]>[CH:1]([C:4]([CH3:22])([N:7]1[C:11](=[O:12])[C:10]2[CH:13]=[CH:14][C:15]3[N:16]([CH3:20])[CH:17]=[CH:18][C:19]=3[C:9]=2[C:8]1=[O:21])[C:5]#[N:6])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 57092295HCID 57092295, 화합물

생성물 1

HCID 53975106HCID 53975106, 화합물수율 11.6%

시약·촉매·용매 2

HCID 178418406HCID 178418406, 화합물촉매HCID 7964Chlorobenzene용매

실험 절차

Activated manganese dioxide (27.0 g, 0.31 0 mol) is added to a solution of 3,3a,4,5,6,8b-hexahydro-a-isopropyl-a,6-dimethyl-1,3-dioxobenzo-[1,2-b:3,4-c']dipyrrole-2(1H)-acetonitrile (51.3 g, 0.167 mol) in chlorobenzene. The reaction mixture is stirred overnight at reflux temperature, cooled and filtered twice through diatomaceous earth with methylene chloride. The filtrate is concentrated in vacuo to a black oil which is flash chromatographed twice with methylene chloride then hexanes:methylene chloride to afford a yellow solid (5.50 g, 11.6%). Recrystallization from hexanes:methylene chloride afforded the title product, mp 123-°128° C.

후처리

  1. temperatureat reflux temperature
  2. temperaturecooled
  3. filtrationfiltered twice through diatomaceous earth with methylene chloride
  4. concentrationThe filtrate is concentrated in vacuo to a black oil which
  5. customchromatographed twice with methylene chloride

출처 및 근거

ORD 기록
ord-28fbc0c174134e0983e4685019662e7f
출처 데이터셋
uspto-grants-1992_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05108485

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