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Phenol → HCID 15016114、化合物

HRID 2226109
ノート
印刷プレビュー

反応式

HRID 2226109 の反応式
[H-].[Na+].[C:3]1([OH:9])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N:18]1[CH2:23][CH2:22][N:21]([C:24](=[O:33])[CH:25](Cl)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:20][CH2:19]1>CN(C=O)C>[CH3:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[N:18]1[CH2:23][CH2:22][N:21]([C:24](=[O:33])[CH:25]([O:9][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)[C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:20][CH2:19]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 996PhenolHCID 24758Sodium hydrideHCID 3622053Piperazine, 1-(chlorophenylacetyl)-4-(2-methoxyphenyl)-

生成物 1

HCID 15016114HCID 15016114、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒3 回

反応条件

温度
0 °C

実験手順

Sodium hydride 80% dispersion in oil (1.7 g) was added to dry DMF (100 ml) under argon. Phenol (3.76 g; 0.04 m) was added over 20 mins and the resulting grey mixture was stirred a further 20 mins and cooled to 0° C. A solution of 1-(2-methoxyphenyl)-4-(1-oxo-2-chloro-2-phenylethyl)piperazine (13.8 g; 0.04 m) in dry DMF (60 ml) was added over 20 mins. The mixture was heated to 60° C. over a period of about 3 hrs and then maintained at 60° C. for 21/2 hrs and then stirred at ambient temperature overnight. The mix was cooled to 0° C., treated with 10 ml crushed ice and the DMF was vacuumed off. The residue, in methylene chloride, was washed well with water and dried over magnesium sulphate. The oil resulting on evaporation, solidified on standing for a few days to give 1-(2-methoxyphenyl)-4 -(1-oxo-2-phenoxy-2-phenylethyl)piperazine.

後処理

  1. temperatureThe mixture was heated to 60° C. over a period of about 3 hrs
  2. temperaturemaintained at 60° C. for 21/2 hrs
  3. stirringstirred at ambient temperature overnight
  4. temperatureThe mix was cooled to 0° C.
  5. additiontreated with 10 ml
  6. customcrushed ice
  7. washThe residue, in methylene chloride, was washed well with water
  8. dry with materialdried over magnesium sulphate
  9. customThe oil resulting on evaporation
  10. waiton standing for a few days

出典と根拠

ORDレコード
ord-acb67f5fcc59479ba99edd53bd79c9ff
出典データセット
uspto-grants-1994_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05346896

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート