Phenyl glycidyl ether → N-[4-[4-(2-hydroxy-3-phenoxypropyl)piperazin-1-yl]phenyl]methanesulfonamide

HRID 728829ノート

反応式

HRID 728829 の反応式
CS(O)(=O)=O.[N:6]1([C:12]2[CH:17]=[CH:16][C:15]([NH:18][S:19]([CH3:22])(=[O:21])=[O:20])=[CH:14][CH:13]=2)[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.[O:23]1[CH:25]([CH2:26][O:27][C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=2)[CH2:24]1.C[O-].[Na+]>CO>[OH:23][CH:25]([CH2:26][O:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)[CH2:24][N:9]1[CH2:10][CH2:11][N:6]([C:12]2[CH:13]=[CH:14][C:15]([NH:18][S:19]([CH3:22])(=[O:21])=[O:20])=[CH:16][CH:17]=2)[CH2:7][CH2:8]1

参加物

5

反応物 3

HCID 31217Phenyl glycidyl etherHCID 10942334Sodium MethoxideHCID 86745083N-[4-(piperazin-1-yl)phenyl]methanesulfonamide methanesulfonate

生成物 1

HCID 14739896N-[4-[4-(2-hydroxy-3-phenoxypropyl)piperazin-1-yl]phenyl]methanesulfonamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
60 °C

実験手順

Suspend a mixture of 20.0 g (56.9 mmol) of N-[4-(piperazin-1-yl)phenyl]methanesulfonamide methanesulfonate, 7.68 mL (56.9 mmol) of 1,2-epoxy-3-phenoxypropane and 3.07 g (56.9 mmol) of sodiummethoxide in 800 mL of 90% aqueous methanol and warm to 60° C. for 18 h. After 18 h, filter the precipitate and wash this precipitate with 100 mL of water and 100 mL of methanol. Suspend this solid precipitate in 500 mL of methanol and reflux for 1 h. After 1 h, cool the suspension to room temperature and filter to obtain the title compound.

後処理

  1. filtrationfilter the precipitate
  2. washwash this precipitate with 100 mL of water and 100 mL of methanol
  3. temperaturereflux for 1 h
  4. waitAfter 1 h
  5. temperaturecool the suspension to room temperature
  6. filtrationfilter

出典と根拠

ORDレコード
ord-e08eaf4769d64f228a4ae5d48c13dfb2
出典データセット
uspto-grants-1991_09
特許番号
US05051423

反応ノート

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