2,3-Dichloro-5,6-dicyano-1,4-benzoquinone → 2-Iodophenanthrene

HRID 68494노트

반응식

HRID 68494 반응식
[I:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][CH2:5][C:4]=2[CH:3]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl>O1CCOCC1>[I:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH:6]=[CH:5][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 576345402-Iodo-9,10-dihydrophenanthrene

생성물 1

HCID 123833792-Iodophenanthrene수율 78.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Under an argonatmosphere, 125 g of 2-iodo-9,10-dihydrophenanthrene, 98 g of 2,3-dichloro-5,6-dicyano-p-benzoquinone, and 1.2 L of 1,4-dioxane were added, and then the mixture was stirred for 24 hours under heating reflux. After having been cooled to room temperature, the reaction solution was concentrated. The residue was purified by silica gel column chromatography, and was then washed with methanol. Thus, 98 g of a white crystal were obtained (in 68% yield).

후처리

  1. temperatureunder heating
  2. temperaturereflux
  3. concentrationthe reaction solution was concentrated
  4. customThe residue was purified by silica gel column chromatography
  5. washwas then washed with methanol

출처 및 근거

ORD 기록
ord-245af911a1244422b6976035c608e6bb
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822041B2

반응 노트

불러오는 중…