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Ammonium Chloride → p-(6-Methoxy-2-phenyl-3,4-dihydro-1-naphthyl)phenol

HRID 1926577
ノート
印刷プレビュー

反応式

HRID 1926577 の反応式
C(O[K])(C)(C)C.[CH3:7][O:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]([C:25]3[CH:30]=[CH:29][C:28]([O:31]C(=O)C(C)(C)C)=[CH:27][CH:26]=3)[CH:14]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH:15]=[CH:16]2)=[CH:11][CH:10]=1.[Cl-].[NH4+]>CS(C)=O>[OH:31][C:28]1[CH:27]=[CH:26][C:25]([C:13]2[C:12]3[C:17](=[CH:18][C:9]([O:8][CH3:7])=[CH:10][CH:11]=3)[CH2:16][CH2:15][C:14]=2[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)=[CH:30][CH:29]=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 25517Ammonium ChlorideHCID 575434947-Methoxy-3-phenyl-4-(4-pivaloyloxyphenyl)-3,4-dihydronaphthaleneHCID 178418922HCID 178418922、化合物

生成物 1

HCID 200362p-(6-Methoxy-2-phenyl-3,4-dihydro-1-naphthyl)phenol収率 69%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

To a dimethyl sulfoxide (0.6 mL) solution of tertiary butoxy potassium (40.3 mg, 0.359 mmol), a dimethyl sulfoxide (0.8 mL) solution of 7-methoxy-3-phenyl-4-(4-pivaloyloxyphenyl)-3,4-dihydronaphthalene (6, 29.3 mg, 0.0710 mmol) was added, and stirred at room temperature for one day and night. After adding saturated ammonium chloride (10 mL) to the reaction mixture with much stirring, extraction was carried out three times with diethyl ether. The organic layers were combined, washed with a saturated sodium chloride solution (10 mL), and after drying with anhydrous sodium sulphate, concentrated. The residue was purified with thin layer chromatography (toluene:ethyl acetate=10:1), to obtain the subject compound (7, 16.0 mg; yield=69%).

後処理

  1. extractionwith much stirring, extraction
  2. washwashed with a saturated sodium chloride solution (10 mL)
  3. dry with materialafter drying with anhydrous sodium sulphate
  4. concentrationconcentrated
  5. customThe residue was purified with thin layer chromatography (toluene:ethyl acetate=10:1)
  6. customto obtain the subject compound (7, 16.0 mg; yield=69%)

出典と根拠

ORDレコード
ord-e271fb3a49d840d492d2df129b62b66b
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08183235B2

反応ノート

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