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(2R,3R)-1-(Dimethylamino)-3-(3-methoxyphenyl)-2-methylpentan-3-ol HCl → (Z)-(RS)-[3-(3-methoxy-phenyl)-2-methyl-pent-3-enyl]-dimethylamine hydrochloride

HRID 2394979
ノート
印刷プレビュー

反応式

HRID 2394979 の反応式
[ClH:1].[CH3:2][N:3]([CH3:19])[CH2:4][CH:5]([CH3:18])[C:6]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=1)(O)[CH2:7][CH3:8]>Cl>[ClH:1].[CH3:17][O:16][C:12]1[CH:11]=[C:10](/[C:6](=[CH:7]\[CH3:8])/[CH:5]([CH3:18])[CH2:4][N:3]([CH3:19])[CH3:2])[CH:15]=[CH:14][CH:13]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 18974517(2R,3R)-1-(Dimethylamino)-3-(3-methoxyphenyl)-2-methylpentan-3-ol HCl

生成物 1

HCID 67662047(Z)-(RS)-[3-(3-methoxy-phenyl)-2-methyl-pent-3-enyl]-dimethylamine hydrochloride収率 42.4%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

200 g (0.69 mole) of hydrochloride (2) were dissolved in one litre of concentrated hydrochloric acid and allowed to stand at room temperature. The hydrochloric acid was removed by distillation under vacuum. The residue was dissolved in 1 l of ice-water and the pH was adjusted to 13 with 10 molar sodium hydroxide solution. After extraction with ether, drying the organic phase and removing the solvent by distillation, 162 g of crude product were obtained, and were purified by recrystallisation. 79 g (42% theoretical) of hydrochloride (1) with a melting point of 169°-170° C. were obtained.

後処理

  1. customto stand at room temperature
  2. customThe hydrochloric acid was removed by distillation under vacuum
  3. dissolutionThe residue was dissolved in 1 l of ice-water
  4. extractionAfter extraction with ether
  5. customdrying the organic phase
  6. customremoving the solvent
  7. distillationby distillation
  8. custom162 g of crude product were obtained
  9. customwere purified by recrystallisation

出典と根拠

ORDレコード
ord-91112e3c564546939c0e202761c1d68f
出典データセット
uspto-grants-1998_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05811582

反応ノート

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