Magnesium Carbonate → 2-(4-Chlorophenyl)selenazole-5-carbaldehyde

HRID 45901

反応式

HRID 45901 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[Se:7])=[CH:4][CH:3]=1.Cl[CH:12]([CH:15]=O)[CH:13]=[O:14].C(=O)([O-])[O-].[Mg+2]>COCCOC>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]2[Se:7][C:12]([CH:13]=[O:14])=[CH:15][N:8]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11029Magnesium CarbonateHCID 147646ChloromalonaldehydeHCID 178514152HCID 178514152、化合物

生成物 1

HCID 595624942-(4-Chlorophenyl)selenazole-5-carbaldehyde収率 59.9%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
60 °C

実験手順

To a suspension of 4-chloroselenobenzamide (219 mg, 1 mmol) and 2-chloromalonaldehyde (160 mg, 1.5 mmol) in 1,2-dimethoxyethane (1.5 ml) is added magnesium carbonate (42 mg, 0.5 mmol) and the resulting mixture is stirred at 60° C. under an atmosphere of nitrogen for 3 hours. The crude reaction mixture is then filtered through a plug of silica and washed with ethyl acetate, and filtrate is concentrated to give a brown solid. The crude product is purified by flash chromatography on silica gel to give 2-(4-chlorophenyl)selenazole-5-carbaldehyde (162 mg).

後処理

  1. customThe crude reaction mixture
  2. filtrationis then filtered through a plug of silica
  3. washwashed with ethyl acetate, and filtrate
  4. concentrationis concentrated
  5. customto give a brown solid
  6. customThe crude product is purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-25dead43989e45ee9be45a561f9127bc
出典データセット
uspto-grants-2013_09
特許番号
US08541594B2

関連ノート

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