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Potassium Iodide → 9-bromo-13,13-dimethyl-6,11-diphenyl-13H-indeno[1,2-b]anthracene

HRID 40409
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인쇄 미리보기

반응식

HRID 40409 반응식
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:12]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)(O)[C:11]3[CH:10]=[C:9]4[C:23]5[C:28]([C:29]([CH3:31])([CH3:30])[C:8]4=[CH:7][C:6]=3[C:5]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)(O)[C:4]=2[CH:3]=1)=[CH:27][CH:26]=[CH:25][CH:24]=5.[I-].[K+].[PH2]([O-])=O.[Na+]>C(O)(=O)C>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[C:5]([C:33]3[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=3)[C:6]3[CH:7]=[C:8]4[C:29]([CH3:30])([CH3:31])[C:28]5[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=5)[C:9]4=[CH:10][C:11]=3[C:12]=2[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 4875Potassium IodideHCID 673867679-bromo-13,13-dimethyl-6,11-diphenyl-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diolHCID 178527019HCID 178527019, 화합물

생성물 1

HCID 866572049-bromo-13,13-dimethyl-6,11-diphenyl-13H-indeno[1,2-b]anthracene수율 74%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

9-bromo-13,13-dimethyl-6,11-diphenyl-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (4.19 g, 0.0075 mol), potassium iodide (12.45 g, 0.075 mol), and sodium hypophosphite (6 g, 0.037 mol) were placed in a flask, and were suspended in acetic acid (200 ml). The reaction mixture was stirred for five hours while heating. After the reaction was terminated, the reaction solution was added to an excess of distilled water. The resultant solid was washed with distilled water, filtered, and purified by column chromatography to give 9-bromo-13,13-dimethyl-6,11-diphenyl-13H-indeno[1,2-b]anthracene (2.9 g, yield=74%).

후처리

  1. temperaturewhile heating
  2. customAfter the reaction was terminated
  3. additionthe reaction solution was added to an excess of distilled water
  4. washThe resultant solid was washed with distilled water
  5. filtrationfiltered
  6. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-325e201e805644599f1aa2cb08829680
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08525158B2

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