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Triethylsilane → 2,3-Dihydro-4,7-dimethoxy-1H-indene

HRID 389295
ノート
印刷プレビュー

反応式

HRID 389295 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]2[C:4]=1[CH2:5][CH2:6][C:7]2=O.C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[CH3:13][O:12][C:9]1[CH:10]=[CH:11][C:3]([O:2][CH3:1])=[C:4]2[C:8]=1[CH2:7][CH2:6][CH2:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12052TriethylsilaneHCID 6060124,7-dimethoxy-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 126541332,3-Dihydro-4,7-dimethoxy-1H-indene

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To the cooled and stirred suspension of 4,7-Dimethoxyindan-1-one (35 gm, 0.182 mole) in Triethyl silane (105.7 gm, 0.909 mole), added Trifluoroacetic acid (350 ml) at 10-15° C. The stirring was continued at room temperature for 2 hours and quenched into the water. It was extracted with Ethyl acetate. The Ethyl acetate layer was washed with Sodium bicarbonate solution, dried over Sodium sulphate and evaporated to give crude mass which was purified by column chouromatography using 5% Ethyl acetate in hexane (22.5 gm).

後処理

  1. temperatureTo the cooled
  2. customquenched into the water
  3. extractionIt was extracted with Ethyl acetate
  4. washThe Ethyl acetate layer was washed with Sodium bicarbonate solution
  5. dry with materialdried over Sodium sulphate
  6. customevaporated
  7. customto give crude mass which
  8. customwas purified by column chouromatography

出典と根拠

ORDレコード
ord-b02e0f252d6443fe8f380246ef849ad5
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08378118B2

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