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Ammonium Chloride → (3RS,4RS)-7-methoxy-3-(4-methoxyphenyl)-4-(2-propenyl)-3-propylthiochroman

HRID 1267780
ノート
印刷プレビュー

反応式

HRID 1267780 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=O)[C:8]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)([CH2:13][CH2:14][CH3:15])[CH2:9][S:10]2)=[CH:5][CH:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl-].[NH4+].[CH2:33]([Si](C)(C)C)[CH:34]=[CH2:35]>O1CCCC1.ClCCCl.[I-].[Zn+2].[I-].O>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH:7]([CH2:35][CH:34]=[CH2:33])[C:8]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][CH:17]=3)([CH2:13][CH2:14][CH3:15])[CH2:9][S:10]2)=[CH:5][CH:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 25517Ammonium ChlorideHCID 69808AllyltrimethylsilaneHCID 18546285HCID 18546285、化合物HCID 21226445Aluminium lithium hydride

生成物 1

HCID 18546273(3RS,4RS)-7-methoxy-3-(4-methoxyphenyl)-4-(2-propenyl)-3-propylthiochroman収率 72.2%

試薬・触媒・溶媒 4

HCID 9883512
zinc(II)iodide
触媒
HCID 111,2-Dichloroethane溶媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 7-methoxy-3-(4-methoxyphenyl)-3-propylthiochroman-4-one (1.7 g, 4.96 mmol) in anhydrous tetrahydrofuran (30 ml) was cooled to −78° C. Lithium aluminum hydride (94.2 mg, 2.48 mmol) was added to this solution, followed by stirring for 12 hours at room temperature. Saturated aqueous ammonium chloride (100 ml) was added to the reaction mixture, which was then extracted twice with ethyl acetate (100 ml). The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, zinc iodide (1.9 g, 5.95 mmol) and allyltrimethylsilane (1.57 ml, 5.95 mmol) were added dropwise to a solution of the residue in 1,2-dichloroethane (50 ml) at 0° C., followed by stirring for 12 hours at room temperature. Water was added to the reaction mixture, which was then extracted twice with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane=1/90) to give (3RS,4RS)-7-methoxy-3-(4-methoxyphenyl)-4-(2-propenyl)-3-propylthiochroman (1.32 g, Yield 72%).

後処理

  1. extractionwas then extracted twice with ethyl acetate (100 ml)
  2. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. stirringby stirring for 12 hours at room temperature
  5. extractionwas then extracted twice with dichloromethane
  6. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationAfter distilling off the solvent
  9. customthe residue was purified by silica gel column chromatography (eluent:ethyl acetate/hexane=1/90)

出典と根拠

ORDレコード
ord-0b008a8629c54ac7bf266a2b976ae13b
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06552068B1

反応ノート

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