Dimethylformamide dimethyl acetal → HCID 67435184、化合物

HRID 1663413ノート

反応式

HRID 1663413 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:13])[CH2:9][C:10](=[O:12])[CH3:11].CO[CH:16](OC)[N:17]([CH3:19])[CH3:18]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:13])[C:9](=[CH:16][N:17]([CH3:19])[CH3:18])[C:10](=[O:12])[CH3:11]

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 149879931-(2-Chlorophenyl)butane-1,3-dione

生成物 1

HCID 67435184HCID 67435184、化合物収率 51%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of crude 1-(2-chlorophenyl)butane-1,3-dione from the previous step and 1,1-dimethoxy-N,N-dimethylmethanamine (2.042 g, 17.14 mmol) in toluene (20 mL) was heated to reflux for 2 h and concentrated. Silica gel chromatography, using 70 to 100% ethyl acetate in hexanes gradient, gave 1-(2-chlorophenyl)-2-((dimethylamino)methylene)butane-1,3-dione as a red, viscous oil (2.20 g, 51% yield for 2 steps). MS (ES+) m/z: 252 (M+H); HPLC retention time: 2.51 min (Analytical HPLC Method D).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 2 h
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-c1a3458a245b47feb21a7ba557415bb9
出典データセット
uspto-grants-2011_10
特許番号
US08034940B2

反応ノート

読み込み中…