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Potassium Iodide → 2-[2-(Benzodioxan-6-yl)ethylamino]-1-(diphenylmethoxy)-2-methylpropane

HRID 1613171
ノート
印刷プレビュー

反応式

HRID 1613171 の反応式
[NH2:1][C:2]([CH3:19])([CH3:18])[CH2:3][O:4][CH:5]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.Br[CH2:21][CH2:22][C:23]1[CH:32]=[CH:31][C:26]2[O:27][CH2:28][CH2:29][O:30][C:25]=2[CH:24]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(#N)C>[O:27]1[C:26]2[CH:31]=[CH:32][C:23]([CH2:22][CH2:21][NH:1][C:2]([CH3:19])([CH3:18])[CH2:3][O:4][CH:5]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=3)=[CH:24][C:25]=2[O:30][CH2:29][CH2:28]1
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 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 190885086-(2-Bromoethyl)-2,3-dihydro-1,4-benzodioxinHCID 197753022-Amino-1-diphenylmethoxy-2-methylpropane

生成物 1

HCID 678852442-[2-(Benzodioxan-6-yl)ethylamino]-1-(diphenylmethoxy)-2-methylpropane

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

実験手順

A mixture of 2-amino-1-diphenylmethoxy-2-methylpropane (369 mg -- see Preparation 1), 6-(2-bromoethyl)benzodioxan (243 mg -- see Preparation 10), potassium carbonate (415 mg) and potassium iodide (166 mg) in acetonitrile (40 ml) was heated under reflux for 48 hours and evaporated. The residue was partitioned between ethyl acetate and water and the organic layer was washed with water, dried over sodium sulphate and evaporated. The residue was purified by chromatography on silica (7 g) using ethyl acetate plus 0-5% methanol as the eluant. Appropriate fractions were combined and evaporated to give the title compound as a colourless oil which was characterised as a hemihydrate (130 mg, 31%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 48 hours
  3. customevaporated
  4. customThe residue was partitioned between ethyl acetate and water
  5. washthe organic layer was washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated
  8. customThe residue was purified by chromatography on silica (7 g)
  9. customevaporated

出典と根拠

ORDレコード
ord-4051eba82e3549c5a6ea136cb7244fbd
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05192765

反応ノート

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