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

HRID 1384841
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HRID 1384841 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

HCID 104886541-(4-Fluoro-2-methoxyphenyl)piperazine수율 25%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매2회

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온도
20 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-c557cffd5cd54ab384ce3a75a9b6c4f2
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06262056B1

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