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HCID 21442569、化合物 → HCID 21442578、化合物

HRID 328526
ノート
印刷プレビュー

反応式

HRID 328526 の反応式
[ClH:1].[CH3:2][C:3]([NH2:19])([CH3:18])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[C:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=1>[Pt](=O)=O.CO>[ClH:1].[CH3:18][C:3]([NH2:19])([CH3:2])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[CH:6][CH:5]=1
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 1

HCID 21442569HCID 21442569、化合物

生成物 1

HCID 21442578HCID 21442578、化合物

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

A mixture of 0.45 gram of α,α-dimethyl-4-(phenylethynyl) -benzylamine hydrochloride, 61 ml. of absolute methanol, and 163 mg. of platinum dioxide catalyst is hydrogenated at 40 p.s.i. for one hour. The hydrogenation is stopped, the catalyst is removed by filtration, and the methanol is removed by evaporation. The residue is partitioned between benzene and 10% sodium hydroxide solution. The benzene phase is washed well with water, dried over magnesium sulfate, filtered, and the benzene is evaporated. The residual oil is dissolved in ether and treated with ethanolic hydrogen chloride. The precipitate is collected and recrystallized from isopropanol and ether to give α,α-dimethyl-4-phenethylbenzylamine hydrochloride, m.p. 225°-228° C.

後処理

  1. customthe catalyst is removed by filtration
  2. customthe methanol is removed by evaporation
  3. customThe residue is partitioned between benzene and 10% sodium hydroxide solution
  4. washThe benzene phase is washed well with water
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customthe benzene is evaporated
  8. dissolutionThe residual oil is dissolved in ether
  9. additiontreated with ethanolic hydrogen chloride
  10. customThe precipitate is collected
  11. customrecrystallized from isopropanol and ether

出典と根拠

ORDレコード
ord-14e2ee66fd734a82a189e188585e983b
出典データセット
uspto-grants-1977_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04017543

反応ノート

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