Sodium Hydroxide → N-[2-Hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine

HRID 486376ノート

反応式

HRID 486376 の反応式
[Cl:1][C:2]1[C:7]([O:8][CH3:9])=[C:6]([O:10][CH3:11])[CH:5]=[CH:4][C:3]=1[CH2:12][CH2:13][NH:14][C:15](=O)[CH:16]([C:18]1[CH:23]=[CH:22][C:21]([O:24][CH3:25])=[CH:20][CH:19]=1)[OH:17].[OH-].[Na+]>C1(C)C=CC=CC=1>[OH:17][CH:16]([C:18]1[CH:19]=[CH:20][C:21]([O:24][CH3:25])=[CH:22][CH:23]=1)[CH2:15][NH:14][CH2:13][CH2:12][C:3]1[CH:4]=[CH:5][C:6]([O:10][CH3:11])=[C:7]([O:8][CH3:9])[C:2]=1[Cl:1]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 13697589N-(2-chloro-3,4-dimethoxyphenylethyl)-4-methoxymandelamide

生成物 1

HCID 3018199N-[2-Hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine収率 77.2%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

10.58 g of N-(2-chloro-3,4-dimethoxyphenylethyl)-4-methoxymandelamide was dissolved in 105.8 ml of toluene. A solution of 16.5 ml of Vitrite in 16.5 ml of toluene was added dropwise to the solution at room temperature. Then the reaction was conducted at 50° C. for 4 hours. After cooling, 100 ml of a 10% NaOH solution was added dropwise thereto and the mixture was left to stand overnight. Crystals thus formed were separated by filtration, washed with water and dried to obtain 7.87 g (yield: 77.2%) of N-[2-hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine.

後処理

  1. temperatureAfter cooling
  2. waitthe mixture was left
  3. waitto stand overnight
  4. customCrystals thus formed
  5. customwere separated by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-faf1dc85e1e34644a7ae2559847a6ac4
出典データセット
uspto-grants-1994_03
特許番号
US05292521

反応ノート

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