Sodium Bicarbonate → 1-(2-Fluoro-5-methylsulfonylphenyl)piperazine

HRID 1792486ノート

反応式

HRID 1792486 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH3:11])(=[O:10])=[O:9])=[CH:4][C:3]=1[NH2:12].Cl.Cl[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]Cl.C(=O)(O)[O-].[Na+]>ClC1C=CC=CC=1Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([CH3:11])(=[O:9])=[O:10])=[CH:4][C:3]=1[N:12]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 522769Bis(2-chloroethyl)amine hydrochlorideHCID 27746372-Fluoro-5-(methylsulfonyl)aniline

生成物 1

HCID 220320111-(2-Fluoro-5-methylsulfonylphenyl)piperazine収率 39%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

10 mL solution of 432 mg 2-fluoro-5-methylsulfonylphenylamine (compound in Production Example 338) and 490 mg bis(2-chloroethyl)amine hydrochloride in 1,2-dichlorobenzene was stirred at 200° C. for 9 hours. The reaction mixture was neutralized by adding an aqueous saturated sodium bicarbonate solution and then extracted with dichloromethane. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed, and the resulting crude product was purified by NH silica gel column chromatography (ethyl acetate/hexane) to give 230 mg of the title compound (dark brown solid).

後処理

  1. extractionextracted with dichloromethane
  2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  3. customthe solvent was removed
  4. customthe resulting crude product was purified by NH silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-301e0a8a384a44118b2bb5ca131ee775
出典データセット
uspto-grants-2006_07
特許番号
US07074801B1

反応ノート

読み込み中…