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Hydrochloric Acid → (R)-1-(4-Chloro-3,5-dimethyl-phenyl)-2-methyl-propylamine hydrochloride

HRID 1629752
ノート
印刷プレビュー

反応式

HRID 1629752 の反応式
[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([C@H:9]([NH:13][S@@](C(C)(C)C)=O)[CH:10]([CH3:12])[CH3:11])=[CH:4][C:3]=1[CH3:20].Cl>CO>[ClH:1].[Cl:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([C@H:9]([NH2:13])[CH:10]([CH3:11])[CH3:12])=[CH:4][C:3]=1[CH3:20]
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 2

HCID 313Hydrochloric AcidHCID 67329434(R)-2-Methyl-propane-2-sulfinic acid [(R)-1-(4-chloro-3,5-dimethyl-phenyl)-2-methyl-propyl]-amide

生成物 1

HCID 67346920(R)-1-(4-Chloro-3,5-dimethyl-phenyl)-2-methyl-propylamine hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of intermediate INT 61 (4.53 g, 14.34 mmol) in MeOH (75 mL) was treated with HCl (4 M in dioxane, 7.17 mL, 28.7 mmol) and stirred overnight. After evaporation of the solvents, a solid was obtained which was washed with Et2O. The solid was then dissolved in 10% sodium carbonate solution and extracted twice with EtOAc. The combined organic layers were dried over sodium sulfate, filtered and concentrated. The crude amine was dissolved in Et2O and treated with an excess of an ethereal solution of HCl (2 M). The suspension was concentrated to yield the title compound.

後処理

  1. customAfter evaporation of the solvents
  2. customa solid was obtained which
  3. washwas washed with Et2O
  4. dissolutionThe solid was then dissolved in 10% sodium carbonate solution
  5. extractionextracted twice with EtOAc
  6. dry with materialThe combined organic layers were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. dissolutionThe crude amine was dissolved in Et2O
  10. additiontreated with an excess of an ethereal solution of HCl (2 M)
  11. concentrationThe suspension was concentrated

出典と根拠

ORDレコード
ord-ffa3c1a60551467f95be3d262370ab3d
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08791100B2

反応ノート

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