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Potassium Carbonate → HCID 10194975、化合物

HRID 397593
ノート
印刷プレビュー

反応式

HRID 397593 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=2)[C:10]2[C:19]3[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=1.C([O-])([O-])=O.[K+].[K+].Cl.ClC[CH2:36][N:37]1[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]1>CC(C)=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([CH:9]([C:20]2[CH:21]=[CH:22][C:23]([O:26][CH2:41][CH2:42][N:37]3[CH2:36][CH2:40][CH2:39][CH2:38]3)=[CH:24][CH:25]=2)[C:10]2[C:19]3[CH2:18][CH2:17][CH2:16][CH2:15][C:14]=3[CH:13]=[CH:12][CH:11]=2)=[CH:5][CH:4]=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 74826Piperidine, 1-(2-chloroethyl)-, hydrochlorideHCID 12114666(4-methoxyphenyl)-(4-hydroxyphenyl)-5,6,7,8-tetrahydronaphth-1-yl-methane

生成物 1

HCID 10194975HCID 10194975、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of (4-methoxyphenyl)-(4-hydroxyphenyl)-5,6,7,8-tetrahydronaphth-1-yl-methane (300 mg, 0.001 mol), anhydrous K2CO3 (2.0 gm, 0.014 mol), 1-(2-chloroethyl)piperidine hydrochloride (300 mg, 0.0015 mol) and dry acetone (25.0 ml) was refluxed for 10 hrs, K2CO3 was filtered off, acetone was distilled off and residue was diluted with water. The reaction mixture was extracted with ethyl acetate, washed with water, dried over sodium sulphate and concentrated to give an oil which was filtered through basic alumina column with benzene as the eluent and concentrated to give the title compound of formula I. Yield 218 mg. (55.89%).

後処理

  1. temperaturewas refluxed for 10 hrs
  2. filtrationK2CO3 was filtered off
  3. distillationacetone was distilled off
  4. additionresidue was diluted with water
  5. extractionThe reaction mixture was extracted with ethyl acetate
  6. washwashed with water
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated
  9. customto give an oil which
  10. filtrationwas filtered through basic alumina column with benzene as the eluent
  11. concentrationconcentrated

出典と根拠

ORDレコード
ord-731869ee22cf4ba7bd52321b38363086
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06610705B1

反応ノート

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