Triethylamine → HCID 86734580、化合物

HRID 597453ノート

反応式

HRID 597453 の反応式
[Cl:1]/[C:2](/[CH3:7])=[CH:3]\[C:4](Cl)=[O:5].[NH2:8][C:9]1[CH:10]=[C:11]([C:15](=[O:19])[CH2:16][CH2:17][CH3:18])[CH:12]=[CH:13][CH:14]=1.C(N(CC)CC)C>O1CCCC1>[C:15]([C:11]1[CH:10]=[C:9]([CH:14]=[CH:13][CH:12]=1)[NH:8][C:4](=[O:5])/[CH:3]=[C:2](\[Cl:1])/[CH3:7])(=[O:19])[CH2:16][CH2:17][CH3:18]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1372881-(3-Aminophenyl)butan-1-oneHCID 12231244HCID 12231244、化合物

生成物 1

HCID 86734580HCID 86734580、化合物収率 49.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

29.2 g of β-chlorocrotonyl chloride were added over one hour at 0° C to a mixture of 31 g of m-amino-butyrophenone 21.2 g of triethylamine and 300 ml of tetrahydrofuran and after stirring for 16 hours at 20° C, the mixture was vacuum filtered. The filtrate was concentrated to dryness and the residue was chromatographed over silica gel to obtain 25 g of m-butyryl-3-chlorocrotonanilide melting at 106° C.

後処理

  1. filtrationfiltered
  2. concentrationThe filtrate was concentrated to dryness
  3. customthe residue was chromatographed over silica gel

出典と根拠

ORDレコード
ord-9438bb52a6ca4506b808cc1c9347f1e7
出典データセット
uspto-grants-1977_03
特許番号
US04014679

反応ノート

読み込み中…