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Sodium Iodide → HCID 15766431、化合物

HRID 375998
ノート
印刷プレビュー

反応式

HRID 375998 の反応式
[C:1]1([N:7]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]3[CH:21]=[CH:20][C:19]([O:22]C)=[CH:18][CH:17]=3)=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.S1(CCCC1)(=O)=O.[I-].[Na+].C[Si](C)(C)Cl>O>[C:1]1([N:7]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:8]2[CH:13]=[CH:12][C:11]([CH2:14][CH2:15][C:16]3[CH:17]=[CH:18][C:19]([OH:22])=[CH:20][CH:21]=3)=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 31347SulfolaneHCID 11211174HCID 11211174、化合物

生成物 1

HCID 15766431HCID 15766431、化合物収率 84.7%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
120 °C

実験手順

A mixture of 38.5 g of the 1-(4-diphenylaminophenyl)-2-(4-methoxyphenyl)ethane prepared in Synthesis Example 1-2, 200 ml of sulfolane, and 45 g of sodium iodide was stirred in a four-neck flask at 120° C. to obtain a solution. The thus obtained solution was cooled to 60° C., and 2 ml of distilled water was added to the solution. 32.6 g of trimethylchlorosilane was then added dropwise to the above solution over a period of 30 minutes. Thus, the reaction was carried out at 60° to 70° C. for three hours. The thus obtained reaction mixture was poured into 500 ml of water, whereby a brown tar was obtained. The thus obtained tar was washed with 200 ml of water several times, and dissolved in 300 ml of toluene, whereby a brown toluene solution was obtained. The thus obtained toluene solution was washed twice with 100 ml of a saturated aqueous solution of sodium sulfite, whereby a transparent toluene solution of light yellow in color was obtained. After the thus obtained transparent toluene solution was dried over anhydrous magnesium sulfate, a solvent was distilled away. The thus obtained product was subjected to chromatography using a silica gel and toluene, whereby 31.4 g of 1-(4-diphenylaminophenyl)-2-(4-hydroxyphenyl)ethane was obtained as an oily material.

後処理

  1. customto obtain a solution
  2. temperatureThe thus obtained solution was cooled to 60° C.
  3. customThe thus obtained reaction mixture
  4. customwas obtained
  5. washThe thus obtained tar was washed with 200 ml of water several times
  6. dissolutiondissolved in 300 ml of toluene
  7. customwhereby a brown toluene solution was obtained
  8. washThe thus obtained toluene solution was washed twice with 100 ml of a saturated aqueous solution of sodium sulfite, whereby a transparent toluene solution of light yellow in color
  9. customwas obtained
  10. dry with materialAfter the thus obtained transparent toluene solution was dried over anhydrous magnesium sulfate
  11. distillationa solvent was distilled away

出典と根拠

ORDレコード
ord-d1bbe803d26b4adc8fd6a8b1734b6758
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05488137

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート