Trityl chloride → 5-Methyl-1-trityl-1H-pyrazole-3-carbaldehyde

HRID 493720ノート

反応式

HRID 493720 の反応式
[CH3:1][C:2]1[NH:6][N:5]=[C:4]([CH:7]=[O:8])[CH:3]=1.C(N(CC)CC)C.Cl[C:17]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(#N)C>[CH3:1][C:2]1[N:6]([C:17]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)([C:30]2[CH:31]=[CH:32][CH:33]=[CH:34][CH:35]=2)[C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)[N:5]=[C:4]([CH:7]=[O:8])[CH:3]=1

参加物

5

反応物 3

HCID 6456Trityl chlorideHCID 8471TriethylamineHCID 45602443-methyl-1H-pyrazole-5-carbaldehyde

生成物 1

HCID 231309495-Methyl-1-trityl-1H-pyrazole-3-carbaldehyde

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 5-methyl-1H-pyrazole-3-carbaldehyde (Werner A. et al., Tetrahedron, 51, 4779 (1995): 1.1 g) in acetonitrile (20 mL), triethylamine (1.5 mL) and chlorotriphenylmethane (3.1 g) were added and mixed for 12 hours. The reaction solution was concentrated, and the residue was dissolved in chloroform. This solution was washed with a saturated aqueous sodium bicarbonate solution and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified with a silica gel column to give the title compound (1.9 g) as a colorless solid.

後処理

  1. additionmixed for 12 hours
  2. concentrationThe reaction solution was concentrated
  3. dissolutionthe residue was dissolved in chloroform
  4. washThis solution was washed with a saturated aqueous sodium bicarbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off
  7. customthe residue was purified with a silica gel column

出典と根拠

ORDレコード
ord-c0df0a26c733414cb6ce24a454ee818a
出典データセット
uspto-grants-2009_05
特許番号
US07534887B2

反応ノート

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