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Water → 1-(4-Fluoro-2-methoxyphenyl)piperazine

HRID 1384841
ノート
印刷プレビュー

反応式

HRID 1384841 の反応式
O.Cl.[F:3][C:4]1[CH:10]=[CH:9][C:7]([NH2:8])=[C:6]([O:11][CH3:12])[CH:5]=1.Cl.Cl[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]Cl>ClC1C=CC=CC=1>[F:3][C:4]1[CH:10]=[CH:9][C:7]([N:8]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)=[C:6]([O:11][CH3:12])[CH:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 522769Bis(2-chloroethyl)amine hydrochlorideHCID 211838464-Fluoro-2-methoxyaniline hydrochloride

生成物 1

HCID 104886541-(4-Fluoro-2-methoxyphenyl)piperazine収率 25%

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒2 回

反応条件

温度
20 °C

実験手順

9 ml of chlorobenzene and H2O were distilled from a solution of 1.14 g of p-TosOH (6.03×10−3 moles) in 200 ml of chlorobenzene. The solution was cooled to 20° C. and then 1.19 g of 4-fluor-2-methoxyaniline hydrochloride (6.7×10−3 moles) and 1.31 g of bis (2-chloroethyl)amine hydrochloride (7.36×10−3 moles) were added. The reaction was held under reflux for 72 hours after which the solvent was removed and the residue was extracted with 5 ml of NaOH 2N and 30 ml of toluene. The organic phase was washed with H2O, was dried with Na2SO4 and the toluene was removed. The product was purified by silica column using dichloromethane/MeOH (9:1) as mobile phase. An oil was obtained. Yield: 25%.

後処理

  1. temperatureunder reflux for 72 hours after which the solvent
  2. customwas removed
  3. extractionthe residue was extracted with 5 ml of NaOH 2N and 30 ml of toluene
  4. washThe organic phase was washed with H2O
  5. dry with materialwas dried with Na2SO4
  6. customthe toluene was removed
  7. customThe product was purified by silica column
  8. customAn oil was obtained

出典と根拠

ORDレコード
ord-c557cffd5cd54ab384ce3a75a9b6c4f2
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06262056B1

反応ノート

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