Chlorotrimethylsilane → [1-(3-Bromo-4-methoxyphenyl)cyclopropyloxy]trimethylsilane

HRID 406396ノート

反応式

HRID 406396 の反応式
[CH3:1][Si:2](Cl)([CH3:4])[CH3:3].[Br:6][C:7]1[CH:8]=[C:9]([C:15]2([OH:18])[CH2:17][CH2:16]2)[CH:10]=[CH:11][C:12]=1[O:13][CH3:14].C(N(CC)CC)C>C1COCC1.O>[Br:6][C:7]1[CH:8]=[C:9]([C:15]2([O:18][Si:2]([CH3:4])([CH3:3])[CH3:1])[CH2:17][CH2:16]2)[CH:10]=[CH:11][C:12]=1[O:13][CH3:14]

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 8471TriethylamineHCID 626698761-(3-Bromo-4-methoxyphenyl)cyclopropanol

生成物 1

HCID 66618984[1-(3-Bromo-4-methoxyphenyl)cyclopropyloxy]trimethylsilane

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Trimethylsilyl chloride (6.54 ml) was added to a solution of 1-(3-bromo-4-methoxyphenyl)cyclopropanol (5.0 g) and triethylamine (8.61 ml) in THF (100 ml). The reaction mixture was stirred at room temperature for 3 days. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to obtain the title compound (3.84 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-012c5307faf646d5a50f18d00ec9ef16
出典データセット
uspto-grants-2014_06
特許番号
US08754100B2

反応ノート

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