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Trityl chloride → HCID 15475336, 화합물

HRID 566238
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HRID 566238 반응식
[NH:1]1[CH:5]=[CH:4][C:3]([CH2:6][CH2:7][OH:8])=[N:2]1.[NH:9]1[CH:13]=[C:12]([CH2:14][CH2:15][OH:16])[CH:11]=[N:10]1.C(N(CC)CC)C.[C:24](Cl)([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>CN(C=O)C.O>[C:25]1([C:24]([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[N:1]2[CH:5]=[CH:4][C:3]([CH2:6][CH2:7][OH:8])=[N:2]2)[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1.[C:25]1([C:24]([C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=2)([C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)[N:9]2[CH:13]=[C:12]([CH2:14][CH2:15][OH:16])[CH:11]=[N:10]2)[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 42936042-(1H-Pyrazol-4-yl)ethanolHCID 178520322HCID 178520322, 화합물

생성물 2

HCID 15475336HCID 15475336, 화합물HCID 154753372-[1-(Triphenylmethyl)-1H-pyrazol-4-yl]ethan-1-ol

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-(3-pyrazolyl)ethanol and 2-(4-pyrazolyl)ethanol (2.4:1) (2.50 g) was dissolved in DMF (30 ml). To the solution were added, while stirring, triethylamine (2.26 g) and trityl chloride (6.22 g). The mixture was stirred at 25° C. for one hour, then at 40° C. for one hour. The reaction mixture was diluted with water, which was subjected to extraction with ethyl acetate. The organic layer was washed with an aqueous saline solution, which was dried over anhydrous magnesium sulfate, followed by concentration under reduced pressure. The concentrate was purified by means of a column chromatography (carrier: silica gel, 300 g, developing solvent: ethyl acetate-hexane, 1:1) to afford 2-(1-triphenylmethyl-3-pyrazolyl)ethanol (3.75 g) and 2-(1-triphenylmethyl-4-pyrazolyl)ethanol (1.42 g).

후처리

  1. additionTo the solution were added
  2. stirringThe mixture was stirred at 25° C. for one hour
  3. extractionwas subjected to extraction with ethyl acetate
  4. washThe organic layer was washed with an aqueous saline solution, which
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. concentrationfollowed by concentration under reduced pressure
  7. customThe concentrate was purified by means of a column chromatography (carrier: silica gel, 300 g, developing solvent: ethyl acetate-hexane, 1:1)

출처 및 근거

ORD 기록
ord-5eb0e8ee898c4b9293039966ec2b7b64
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06174877B1

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