Dimethylformamide → HCID 54001055、化合物

HRID 1489390ノート

反応式

HRID 1489390 の反応式
C(=O)([O-])[O-].[K+].[K+].[CH2:7](Cl)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.CN(C=O)C.[Cl:20][C:21]1[CH:42]=[CH:41][C:24]([CH2:25][O:26][C:27]2[CH:40]=[CH:39][CH:38]=[CH:37][C:28]=2[C:29]([N:32]2[CH:36]=[CH:35][N:34]=[CH:33]2)=[N:30][OH:31])=[CH:23][CH:22]=1>CCOCC>[CH2:7]([O:31][N:30]=[C:29]([N:32]1[CH:36]=[CH:35][N:34]=[CH:33]1)[C:28]1[CH:37]=[CH:38][CH:39]=[CH:40][C:27]=1[O:26][CH2:25][C:24]1[CH:41]=[CH:42][C:21]([Cl:20])=[CH:22][CH:23]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 74003411HCID 74003411、化合物

生成物 1

HCID 54001055HCID 54001055、化合物収率 90.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

Potassium carbonate (0.21 g), benzyl chloride (0.15 g) and DMF (2 ml) were added to 2-(4-chlorobenzyloxy)-α-(1-imidazolyl)benzaldehyde oxime (0.33 g), and the mixture was stirred at 60° C. for 2 hours. After completion of the reaction, ether (100 ml) was added, and the mixture was extracted with brine (80 ml) twice, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting crude product was purified by silica gel chromatography to give 2-(4-chlorobenzyloxy)-α-(1-imidazolyl)benzaldehyde O-benzyloxime (0.38 g) as colorless crystals. mp. 94°-95.5° C.

後処理

  1. additionwas added
  2. extractionthe mixture was extracted with brine (80 ml) twice
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting crude product was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-acfa8e6df3ab4c248431f728d3925e7f
出典データセット
uspto-grants-1997_10
特許番号
US05677465

反応ノート

読み込み中…