N-bromobutanimide → HCID 67125220、化合物

HRID 1958084ノート

反応式

HRID 1958084 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][N:11]=[C:10]([CH3:19])[N:9]=1.[Br:20]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl>[Br:20][CH2:19][C:10]1[N:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])[C:13]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:12][N:11]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 18981952Ethyl 4-(2-chlorophenyl)-2-methylpyrimidine-5-carboxylate

生成物 1

HCID 67125220HCID 67125220、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

実験手順

An amount of 820 mg (2.96 mmol) of ethyl 4-(2-chlorophenyl)-2-methylpyrimidine-5-carboxylate and 633 mg (3.55 mmol) of N-bromosuccinimide were dissolved in 18 ml of carbon tetrachloride and heated with stirring to boiling. At the heat of boiling, in portions, 49 mg (0.29 mmol) of 2,2′-azobis-2-methylpropanenitrile were added over 5 hours, followed by refluxing for a further hour. After cooling to room temperature, the reaction solution was filtered and the mother liquor was freed from the solvent under reduced pressure. The desired product was isolated by chromatographic purification.

後処理

  1. temperatureheated
  2. temperatureAt the heat
  3. additionwere added over 5 hours
  4. temperatureby refluxing for a further hour
  5. filtrationthe reaction solution was filtered

出典と根拠

ORDレコード
ord-cc4bbd6aafed4497bed39242722ecd9e
出典データセット
uspto-grants-2013_04
特許番号
US08410106B2

反応ノート

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