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

HRID 585360
ノート
印刷プレビュー

反応式

HRID 585360 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 177AcetaldehydeHCID 6115AnilineHCID 178418385HCID 178418385、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-ba7c3a2297f742eda8f932ab40a65b8b
出典データセット
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06930104B2

反応ノート

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