N-bromobutanimide → HCID 67125220、化合物

HRID 874184ノート

反応式

HRID 874184 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

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, with stirring, heated to the boil. At boiling point, 49 mg (0.29 mmol) of 2,2′-azobis-2-methylpropionitrile were added a little at a time over a period of 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 to the boil
  2. additionwere added a little at a time over a period of 5 hours
  3. temperatureby refluxing for a further hour
  4. filtrationthe reaction solution was filtered

出典と根拠

ORDレコード
ord-f560c7d869f14d1fb147ae7209bc58bf
出典データセット
uspto-grants-2015_03
特許番号
US08980886B2

反応ノート

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