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Potassium Carbonate → HCID 66765807、化合物

HRID 556773
ノート
印刷プレビュー

反応式

HRID 556773 の反応式
[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][CH:7]=[C:8]([C:9](=O)[CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1.C([SiH](CC)CC)C.C(=O)([O-])[O-].[K+].[K+]>FC(F)(F)C(O)=O>[Br:1][C:2]1[CH:19]=[CH:18][C:5]2[S:6][CH:7]=[C:8]([CH2:9][CH2:10][C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[C:4]=2[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12052TriethylsilaneHCID 23154554HCID 23154554、化合物

生成物 1

HCID 66765807HCID 66765807、化合物収率 89.2%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To a mixture of 1-(5-bromobenzo[b]thiophen-3-yl)-2-phenylethanone (1.1 g) and triethylsilane (1.5 g) was added trifluoro acetic acid (10 mL) at room temperature, and the mixture was stirred at room temperature for 2 hours. The reaction mixture was poured into an ice-cooled saturated potassium carbonate aqueous solution, and the mixture was extracted with diethyl ether. The organic layer washed with water and brine and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane) to give the title compound (0.94 g).

後処理

  1. extractionthe mixture was extracted with diethyl ether
  2. washThe organic layer washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: n-hexane)

出典と根拠

ORDレコード
ord-65d80e0f8c8443269546211a9f251803
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058245B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート