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

HRID 493720노트

반응식

HRID 493720 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c0df0a26c733414cb6ce24a454ee818a
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534887B2

반응 노트

불러오는 중…