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Hydrochloric Acid → Bis(2-methyl-3-phenyl-1H-inden-7-yl) sulfide

HRID 2357868
ノート
印刷プレビュー

反応式

HRID 2357868 の反応式
[CH3:1][CH:2]1[CH2:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][C:8]=2[S:11][C:12]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:13]=2[CH2:14][CH:15]([CH3:22])[C:16]3=O)[C:3]1=O.[C:24]1([Mg]Br)[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[Mg].Br[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1.Cl>CCOCC.O>[CH3:1][C:2]1[CH2:10][C:9]2[C:4]([C:3]=1[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[CH:5][CH:6]=[CH:7][C:8]=2[S:11][C:12]1[CH:20]=[CH:19][CH:18]=[C:17]2[C:13]=1[CH2:14][C:15]([CH3:22])=[C:16]2[C:34]1[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=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

8

反応物 5

HCID 313Hydrochloric AcidHCID 7961BromobenzeneHCID 5462224MagnesiumHCID 588977942-methyl-4-[(2-methyl-1-oxo-2,3-dihydro-1H-inden-4-yl)sulfanyl]-1-indanoneHCID 178418255HCID 178418255、化合物

生成物 1

HCID 58897800Bis(2-methyl-3-phenyl-1H-inden-7-yl) sulfide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
0 °C

実験手順

Under an argon atmosphere, to a solution of 3.20 g (9.93 mmol) of 2-methyl-4-[(2-methyl-1-oxo-2,3-dihydro-1H-inden-4-yl)sulfanyl]-1-indanone in 20 ml of ether, a solution of PhMgBr in ether [obtained from 0.73 g (30.0 mmol) of magnesium turnings, 4.77 g (30.4 mmol) of bromobenzene, and 30 ml of ether] was added dropwise with vigorous stirring at 0° C. This mixture was stirred overnight and then added to 50 ml of water. Then, to this mixture 12 M HCl (to pH 1) was added. The organic layer was separated; and the aqueous layer was extracted with 3×20 ml of dichloromethane. The combined extract was evaporated, and a mixture of the residue and 0.5 g para-toluenesulfonic acid in 150 ml benzene was refluxed for 1 hour. The resulting mixture was washed with 50 ml of saturated aqueous NaHCO3. The organic layer was separated, dried over Na2SO4, and evaporated to dryness. The product was isolated by flash chromatography on Silica Gel 60 (40-63 μm, d 35 mm, l 300 mm, eluant: hexanes-CH2Cl2=1:2, vol.). Yield, 2.20 g (50%) of a yellowish solid.

後処理

  1. stirringThis mixture was stirred overnight
  2. customThe organic layer was separated
  3. extractionand the aqueous layer was extracted with 3×20 ml of dichloromethane
  4. extractionThe combined extract
  5. customwas evaporated
  6. additiona mixture of the residue and 0.5 g para-toluenesulfonic acid in 150 ml benzene
  7. temperaturewas refluxed for 1 hour
  8. washThe resulting mixture was washed with 50 ml of saturated aqueous NaHCO3
  9. customThe organic layer was separated
  10. dry with materialdried over Na2SO4
  11. customevaporated to dryness
  12. customThe product was isolated by flash chromatography on Silica Gel 60 (40-63 μm, d 35 mm, l 300 mm, eluant: hexanes-CH2Cl2=1:2, vol.)
  13. customYield

出典と根拠

ORDレコード
ord-d44296ed4d704db3a0c32e34abadeead
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07763562B2

反応ノート

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