Potassium Hydroxide → 1-(2-Fluoro-6-methoxyphenyl)piperazine

HRID 1533859ノート

反応式

HRID 1533859 の反応式
[F:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:3]=1[NH2:4].Br.Br[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]Br.[OH-].[K+].[OH-].[Na+]>O>[F:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([O:9][CH3:10])[C:3]=1[N:4]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1

参加物

6

反応物 4

HCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 4592532-Fluoro-6-methoxyanilineHCID 12692731Ethanamine, 2-bromo-N-(2-bromoethyl)-, hydrobromide (1:1)

生成物 1

HCID 156761211-(2-Fluoro-6-methoxyphenyl)piperazine収率 77%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

2-Fluoro-6-methoxyaniline (7.80 g) and 17.23 g of di-(2-bromoethyl)amine hydrobromide were dissolved in 5 ml of water and, by heating at about 110° C. on a bath, 10 ml of 30% potassium hydroxide solution was added thereto (each about 3.5 ml once an hour). Heating was further continued (7 hours in total). After cooled, the reaction solution was made alkaline with aqueous solution of sodium hydroxide to salt out and extracted with chloroform twice. The extract was washed with saturated sodium chloride solution, dried over sodium sulfate, the solvent was evaporated therefrom, and the residue was purified by a column chromatography to give 8.95 g of oily 1-(2-fluoro-6-methoxyphenyl)piperazine in 34.93 g yield or 94%.

後処理

  1. customeach about 3.5 ml once an hour
  2. temperatureHeating
  3. custom(7 hours in total)
  4. temperatureAfter cooled
  5. extractionextracted with chloroform twice
  6. washThe extract was washed with saturated sodium chloride solution
  7. dry with materialdried over sodium sulfate
  8. customthe solvent was evaporated
  9. customthe residue was purified by a column chromatography

出典と根拠

ORDレコード
ord-4221356c531047a2a9f8568c1e0db29d
出典データセット
uspto-grants-1992_02
特許番号
US05086049

反応ノート

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