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Trityl chloride → HCID 15475336、化合物

HRID 566238
ノート
印刷プレビュー

反応式

HRID 566238 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 42936042-(1H-Pyrazol-4-yl)ethanolHCID 178520322HCID 178520322、化合物

生成物 2

HCID 15475336HCID 15475336、化合物HCID 154753372-[1-(Triphenylmethyl)-1H-pyrazol-4-yl]ethan-1-ol

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-5eb0e8ee898c4b9293039966ec2b7b64
出典データセット
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06174877B1

反応ノート

読み込み中…

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