Ethanol → 4-(4-(Methylsulfonyl)piperazin-1-yl)phenol

HRID 2198526ノート

反応式

HRID 2198526 の反応式
Br.Br.[N:3]1([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.C(O)C.C(=O)([O-])O.[Na+].[CH3:24][S:25](Cl)(=[O:27])=[O:26]>O>[OH:15][C:12]1[CH:11]=[CH:10][C:9]([N:3]2[CH2:4][CH2:5][N:6]([S:25]([CH3:24])(=[O:27])=[O:26])[CH2:7][CH2:8]2)=[CH:14][CH:13]=1

参加物

6

反応物 4

HCID 702EthanolHCID 31297Methanesulfonyl chlorideHCID 516892Sodium BicarbonateHCID 2723591p-(1-Piperazinyl)phenol dihydrobromide

生成物 1

HCID 6400494-(4-(Methylsulfonyl)piperazin-1-yl)phenol

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred mixture of 12.9 parts of 4-(1-piperazinyl)-phenol dihydrobromide, 40 parts of ethanol and 50 parts of water are added 12.6 parts of sodium hydrogen carbonate. Then there are added dropwise 6.4 parts of methanesulfonyl chloride at 0° C. Upon completion, stirring is continued overnight. The precipitated product is filtered off and taken up in water. The whole is alkalized with a sodium hydroxide solution and stirred for 30 minutes at room temperature. The mixture is filtered over hyflo and the filtrate is acidified with acetic acid. The precipitated product is filtered off and dried, yielding 2.8 parts of 1-(4-hydroxyphenyl)-4-(methylsulfonyl)-piperazine; mp. 204.9° C.

後処理

  1. filtrationThe precipitated product is filtered off
  2. stirringstirred for 30 minutes at room temperature
  3. filtrationThe mixture is filtered over hyflo
  4. filtrationThe precipitated product is filtered off
  5. customdried

出典と根拠

ORDレコード
ord-ec80264623f1485e9509d3d39ae6ff60
出典データセット
uspto-grants-1982_11
特許番号
US04358449

反応ノート

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