Potassium Iodide → 2-Bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-13h-indeno[1,2-b]anthracene

HRID 1945361ノート

反応式

HRID 1945361 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[C:42](=[CH:43][CH:44]=1)[C:7]1=[CH:8][C:9]3[C:10]([C:32]4[CH:41]=[CH:40][C:39]5[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=5)[CH:33]=4)(O)[C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:16]=4[C:17]([C:21]4[CH:30]=[CH:29][C:28]5[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=5)[CH:22]=4)(O)[C:18]=3[CH:19]=[C:6]1[C:5]2([CH3:46])[CH3:45].[I-].[K+].[PH2]([O-])=O.[Na+]>C(O)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:42](=[CH:43][CH:44]=1)[C:7]1=[CH:8][C:9]3[C:10]([C:32]4[CH:41]=[CH:40][C:39]5[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=5)[CH:33]=4)=[C:11]4[C:16](=[C:17]([C:21]5[CH:30]=[CH:29][C:28]6[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=6)[CH:22]=5)[C:18]=3[CH:19]=[C:6]1[C:5]2([CH3:46])[CH3:45])[CH:15]=[CH:14][CH:13]=[CH:12]4

参加物

5

反応物 3

HCID 4875Potassium IodideHCID 581754872-Bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diolHCID 178527019HCID 178527019、化合物

生成物 1

HCID 581755502-Bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-13h-indeno[1,2-b]anthracene収率 76%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

2-Bromo-13,13-dimethyl-6,11-di(naphthalen-2-yl)-11,13-dihydro-6H-indeno[1,2-b]anthracene-6,11-diol (5 g, 1 eq, 0.0075 mol), potassium iodide (12.45 g, 10 eq, 0.075 mol), and sodium hypophosphite (6 g, 5 eq, 0.037 mol) were placed in a flask, and acetic acid (200 ml) was added thereto. 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, filtered, and purified by column chromatography to give a target compound (3.56 g, yield=76%).

後処理

  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
  5. filtrationfiltered
  6. custompurified by column chromatography

出典と根拠

ORDレコード
ord-75e49b012ecd4ca48f50631dd1b7437e
出典データセット
uspto-grants-2013_03
特許番号
US08395144B2

反応ノート

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