Hydrochloric Acid → 1405433-13-7

HRID 1777744ノート

反応式

HRID 1777744 の反応式
Cl.[NH:2]([CH2:4][C:5]([O:7]CC)=[O:6])[NH2:3].CN(C)/[CH:12]=[CH:13]/[C:14]([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=O.C([O-])([O-])=O.[K+].[K+].Cl>CCO.CC(=O)OCC>[C:16]1([C:14]2[N:2]([CH2:4][C:5]([OH:7])=[O:6])[N:3]=[CH:12][CH:13]=2)[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 5398495(E)-3-Dimethylamino-1-phenyl-propenoneHCID 11593468Acetic acid, 2-hydrazinyl-, ethyl ester, hydrochloride (1:1)

生成物 1

HCID 216451761405433-13-7収率 63.6%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

To a solution of ethyl hydrazinoacetate hydrochloride (866 mg) in EtOH (20 mL) was added (E)-3-(dimethylamino)-1-phenylprop-2-en-1-one (981 mg) and K2CO3 (774 mg). The reaction mixture was stirred at 80° C. for 20 h, cooled down and the pH was brought to 2-3 by adding 1M HCl. EA was added and the phases were separated. The org. layer was washed with brine, dried (Na2SO4) and evaporated in vacuo to afford 720 mg of white solid. LC-MS (B): tR=0.63 min; [M+H]+: 203.43.

後処理

  1. temperaturecooled down
  2. customthe phases were separated
  3. washlayer was washed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-7462d79b031f4d2aa6504aebb6d92cef
出典データセット
uspto-grants-2016_02
特許番号
US09266876B2

反応ノート

読み込み中…