Dimethylformamide → HCID 178502648、化合物

HRID 279456ノート

反応式

HRID 279456 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].[Cl-].[NH4+].CN(C)C=O.[CH3:12][C:13]1[CH:32]=[CH:31][C:30]([CH3:33])=[CH:29][C:14]=1[O:15][CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[C:23](=[N:26][O:27][CH3:28])[C:24]#[N:25]>C(OCC)(=O)C>[CH3:28][O:27][N:26]=[C:23]([C:24]1[NH:25][N:3]=[N:2][N:1]=1)[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[CH2:16][O:15][C:14]1[CH:29]=[C:30]([CH3:33])[CH:31]=[CH:32][C:13]=1[CH3:12]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 54390956HCID 54390956、化合物

生成物 1

HCID 178502648HCID 178502648、化合物収率 87.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
115 °C

実験手順

Sodium azide (1.30 g, 20 mmol), ammonium chloride (1.07 g, 20 mmol) and dimethylformamide (10 ml) were added to 2-(2,5-dimethylphenoxymethyl)-α-methoxyiminophenylacetonitrile (0.59 g, 2 mmol), and the mixture was stirred at 115° C. for 9 hours. After completion of the reaction, ethyl acetate (150 ml) was added, and the mixture was washed with saturated brine (100 ml) twice. The ethyl acetate layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give 2-(2,5-dimethylphenoxymethyl)phenyl 1H-tetrazol-5-yl ketone O-methyloxime (0.59 g, 87.4%) as colorless crystals.

後処理

  1. additionwas added
  2. washthe mixture was washed with saturated brine (100 ml) twice
  3. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate/n-hexane

出典と根拠

ORDレコード
ord-b9351070cde5438abdc2474e7f6a50a5
出典データセット
uspto-grants-2002_03
特許番号
US06362212B1

反応ノート

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