Monobenzone → 1-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine

HRID 894970ノート

反応式

HRID 894970 の反応式
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][N:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH2:21][CH2:20]1>CS(C)=O.[OH-].[Na+]>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:15][CH2:17][CH2:18][N:19]2[CH2:24][CH2:23][N:22]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:21][CH2:20]2)=[CH:13][CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 2

HCID 7638MonobenzoneHCID 47418781-(2-Chloroethyl)-4-phenylpiperazine

生成物 1

HCID 129411031-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 14798Sodium Hydroxide溶媒2 回

実験手順

26.25 ml 4 N NaOH (.105 mol) was added to a stirred mixture of 21.0 g (0.105 mol) 4-benzyloxyphenol and 22.5 g (0.1 mol) of 1-(2-chloroethyl)-4-phenylpiperazine in 250 ml DMSO and the reaction was heated at 60° for 60 min. After cooling, the stirred mixture was diluted with 50 ml 1 N NaOH solution and the resulting crystalline precipitate was collected by filtration and washed with water to give, after drying in vacuo, essentially pure end product, mp 116°-119°.

後処理

  1. temperaturethe reaction was heated at 60° for 60 min
  2. temperatureAfter cooling
  3. filtrationthe resulting crystalline precipitate was collected by filtration
  4. washwashed with water
  5. customto give
  6. customafter drying in vacuo, essentially pure end product, mp 116°-119°

出典と根拠

ORDレコード
ord-b470df3689434c34bdd3071a8273085e
出典データセット
uspto-grants-1981_08
特許番号
US04285873

反応ノート

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