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Sodium Hydroxide → 3-Ethoxy-5-methoxy-2-methyl-1H-indene

HRID 1577038
ノート
印刷プレビュー

反応式

HRID 1577038 の反応式
[CH3:1][O:2][C:3]1[CH:11]=[C:10]2[C:6]([CH2:7][CH:8]([CH3:13])[C:9]2=[O:12])=[CH:5][CH:4]=1.[CH2:14](OC(OCC)OCC)[CH3:15].[OH-].[Na+]>C(O)C.CCOCC>[CH3:13][C:8]1[CH2:7][C:6]2[C:10]([C:9]=1[O:12][CH2:14][CH3:15])=[CH:11][C:3]([O:2][CH3:1])=[CH:4][CH: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

6

反応物 3

HCID 14798Sodium HydroxideHCID 31214Ethyl orthoformateHCID 2311786-Methoxy-2-methyl-2,3-dihydro-1H-inden-1-one

生成物 1

HCID 213953003-Ethoxy-5-methoxy-2-methyl-1H-indene

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

6-Methoxy-2-methylindanone [1.76 g (0.01 mole)] is dissolved in 6.5 ml of absolute ethanol (containing 20% anhydrous ether). This solution is stirred with 2.4 g (0.016 mole) of triethylorthoformate and a drop of redistilled BF3C2H5O C2H5 for about 72 hours. The reaction mixture is diluted with ether, poured slowly into 8.1 ml of 5.0% sodium hydroxide solution with crushed ice with stirring. Two layers separate and the organic layer is washed with cold water until neutral followed by saturated sodium chloride solution and dried over sodium sulfate. This is then filtered and the solvent removed and the residue distilled with 1 ml of benzene solution which contains about 47.5 mg of anhydrous p-toluene sulfonic acid to obtain 2-methyl-3-ethoxy-5-methoxyindene.

後処理

  1. customTwo layers separate
  2. washthe organic layer is washed with cold water
  3. dry with materialdried over sodium sulfate
  4. filtrationThis is then filtered
  5. customthe solvent removed
  6. distillationthe residue distilled with 1 ml of benzene solution which

出典と根拠

ORDレコード
ord-91e8b4682ef548faaf6f4b9e5eebac1b
出典データセット
uspto-grants-1976_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03983253

反応ノート

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