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p-(Trifluoromethoxy)benzaldehyde → 4-[4-(4-Trifluoromethoxybenzyl)piperazin-1-yl]phenol

HRID 856096
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HRID 856096 반응식
[OH:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[F:14][C:15]([F:26])([F:25])[O:16][C:17]1[CH:24]=[CH:23][C:20]([CH:21]=O)=[CH:19][CH:18]=1.C([BH3-])#N.[Na+].C(=O)([O-])O.[Na+]>CO.C(Cl)Cl.C(O)(=O)C>[F:14][C:15]([F:25])([F:26])[O:16][C:17]1[CH:24]=[CH:23][C:20]([CH2:21][N:11]2[CH2:12][CH2:13][N:8]([C:5]3[CH:4]=[CH:3][C:2]([OH:1])=[CH:7][CH:6]=3)[CH2:9][CH2:10]2)=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 69573p-(Trifluoromethoxy)benzaldehydeHCID 92467p-(1-Piperazinyl)phenolHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 307469694-[4-(4-Trifluoromethoxybenzyl)piperazin-1-yl]phenol수율 57%

시약·촉매·용매 3

HCID 176
Acetic Acid
용매
HCID 887Methanol용매
HCID 6344Dichloromethane용매2회

실험 절차

4-(4-hydroxyphenyl)piperazine (3 g, 16.8 mmol) and 4-trifluoromethoxy benzaldehyde (3.36 g, 17.7 mmol) were dissolved in methanol (60 ml) and methylene chloride (15 ml). Sodium cyanoborohydride (1.59 g, 25.3 mmol) and-acetic acid (1.6 ml) were added to this solution while cooling in an ice-bath, and the mixture was stirred for 2 hours. Saturated sodium hydrogencarbonate aqueous solution and methylene chloride were added to the reaction mixture, which was extracted with methylene chloride. The extract was washed with brine, dried over magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (methylene chloride/methanol=100/1) to afford 4-[4-(4-trifluoromethoxybenzyl)piperazin-1-yl]phenol (3.36 g, yield 57%) as a colorless crystalline powder.

후처리

  1. temperaturewhile cooling in an ice-bath
  2. extractionwas extracted with methylene chloride
  3. washThe extract was washed with brine
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (methylene chloride/methanol=100/1)

출처 및 근거

ORD 기록
ord-639556ef32674948b8fae09e68ed14b9
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262212B2

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