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Acetaldehyde → alpha-Methyl-N-phenyl-1H-benzotriazole-1-methanamine

HRID 585360
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HRID 585360 반응식
[NH:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.[NH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[CH:17](=O)[CH3:18]>C(OCC)C>[CH3:17][CH:18]([N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1)[NH:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 177AcetaldehydeHCID 6115AnilineHCID 178418385HCID 178418385, 화합물

생성물 1

HCID 3451461alpha-Methyl-N-phenyl-1H-benzotriazole-1-methanamine수율 93.6%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

In the published manner (J. Org Chem. 1995, 60, 3993), benzotriazole (11.9 g, 100 mmol) and aniline (9.1 ml, 100 mmol) were dissolved in diethyl ether (200 ml), and acetaldehyde (6.1 ml, 110 mmol) was added dropwise thereto on ice. The reaction mixture was stirred at room temperature for 15 minutes and then allowed to stand overnight at −20° C. The crystallized product was collected by filtration, washed with diethyl ether and then dried to give α-methyl-N-phenyl-1H-benzotriazole-1-methanamine (22.3 g) as a white crystal. The resulting α-methyl-N-phenyl-1H-benzotriazole-1-methanamine (2.31 g, 10 mmol) and 9-vinylcarbazole (1.93 g, 10 mmol) were suspended in chloroform (10 ml), to which p-toluenesulfonic acid monohydrate (20 mg, 0.105 mmol) was then added and stirred at room temperature for 2 hours. After addition of water, the reaction mixture was extracted with chloroform. The organic layer was washed with 10% aqueous sodium carbonate and water, and then concentrated. The residue was applied to silica gel column chromatography (developing solvent: ethyl acetate/hexane=1/10) to give the titled compound (644 mg, yield over 2 steps: 20%) as a white crystal.

후처리

  1. waitto stand overnight at −20° C
  2. filtrationThe crystallized product was collected by filtration
  3. washwashed with diethyl ether
  4. customdried

출처 및 근거

ORD 기록
ord-ba7c3a2297f742eda8f932ab40a65b8b
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06930104B2

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