Hydrochloric Acid → HCID 12394366、化合物

HRID 1255812

反応式

HRID 1255812 の反応式
[N+:1]([C:4]1[CH:5]=[C:6](/[CH:10]=[CH:11]/[C:12]([O:14][CH3:15])=[O:13])[CH:7]=[CH:8][CH:9]=1)([O-])=O.Cl>CCO.[Fe]>[NH2:1][C:4]1[CH:5]=[C:6](/[CH:10]=[CH:11]/[C:12]([O:14][CH3:15])=[O:13])[CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 5354136Methyl (2E)-3-(3-nitrophenyl)-2-propenoate

生成物 1

HCID 12394366HCID 12394366、化合物収率 57%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

実験手順

A solution of (E)-methyl 3-(3-nitrophenyl)acrylate (20.14 g, 0.097 mol), Fe (32.5 g, 0.58 mol), concentrated HCl (3.5 ml) in 50% EtOH (100 ml) was refluxed for 2 h. Upon completion, the solution was filtered through Celite and washed with EtOH. The filtrate was concentrated and extracted with dichloromethane. The combined organic phase was dried over MgSO4 and concentrated to afford (E)-methyl 3-(3-aminophenyl)acrylate as a yellow solid (9.73 g, 57%).

後処理

  1. filtrationUpon completion, the solution was filtered through Celite
  2. washwashed with EtOH
  3. concentrationThe filtrate was concentrated
  4. extractionextracted with dichloromethane
  5. dry with materialThe combined organic phase was dried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-23aa94ce1d194a229de0a8a67b963dde
出典データセット
uspto-grants-2013_06
特許番号
US08461157B2

関連ノート

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