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Sodium Chloride → (3S,4S)-7-methoxy-3-(4-methoxyphenyl)-3-methyl-4-(2-propenyl)thiochroman

HRID 398075
ノート
印刷プレビュー

反応式

HRID 398075 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7](=O)[C@:8]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)([CH3:13])[CH2:9][S:10]2)=[CH:5][CH:4]=1.[BH4-].[Na+].[Cl-].[Na+].[CH2:27]([Si](C)(C)C)[CH:28]=[CH2:29]>O1CCCC1.C(O)C.ClCCl.[I-].[Zn+2].[I-].O.CO>[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([C@@H:7]([CH2:29][CH:28]=[CH2:27])[C@:8]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)([CH3:13])[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

11

反応物 4

HCID 5234Sodium ChlorideHCID 69808AllyltrimethylsilaneHCID 4311764Sodium borohydrideHCID 12043768(3R)-7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one

生成物 1

HCID 12043773(3S,4S)-7-methoxy-3-(4-methoxyphenyl)-3-methyl-4-(2-propenyl)thiochroman収率 58.3%

試薬・触媒・溶媒 6

HCID 9883512
zinc(II)iodide
触媒
HCID 702Ethanol溶媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒2 回
HCID 8028Tetrahydrofuran溶媒

実験手順

The (3R)-7-methoxy-3-(4-methoxyphenyl)-3-methylthiochroman-4-one prepared in Example 1 (11.4 g, 36.26 mmol) was dissolved in tetrahydrofuran (40 ml) and ethanol (20 ml). To this solution, sodium borohydride (2.74 g, 72.51 mmol) was added at −78° C., and the resulting mixture was stirred for 15 hours at room temperature. After the reaction was completed, dichloromethane, methanol and saturated aqueous sodium chloride were added to the reaction mixture, which was then extracted under heating conditions. The organic layer was dried over anhydrous magnesium sulfate. After distilling off the solvent, allyltrimethylsilane (10.74 ml, 67.6 mmol) and zinc iodide (12.9 g, 40.57 mmol) were added to a solution of the residue in dichloromethane (300 ml) followed by stirring for 15 hours at room temperature. Water was added to the reaction mixture, which was then extracted with dichloromethane. The organic layer was washed with saturated aqueous ammonium chloride and dried over anhydrous magnesium sulfate, and the resulting residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/90) to give (3S,4S)-7-methoxy-3-(4-methoxyphenyl)-3-methyl-4-(2-propenyl)thiochroman (7.2 g, Yield 58%) as an oil.

後処理

  1. extractionwas then extracted under heating conditions
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. stirringby stirring for 15 hours at room temperature
  4. extractionwas then extracted with dichloromethane
  5. washThe organic layer was washed with saturated aqueous ammonium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe resulting 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-facc9632297d4ab782f470fd52227e34
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06610733B2

反応ノート

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