Diethyl (ethoxymethylene)malonate → Diethyl 2-((2-bromo-4-cyanophenylamino)methylene)malonate

HRID 2367655ノート

反応式

HRID 2367655 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[Br:10].C(O[CH:14]=[C:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])C>C1(C)C=CC=CC=1>[Br:10][C:3]1[CH:4]=[C:5]([C:6]#[N:7])[CH:8]=[CH:9][C:2]=1[NH:1][CH:14]=[C:15]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:21]([O:23][CH2:24][CH3:25])=[O:22]

参加物

4

反応物 2

HCID 6871Diethyl (ethoxymethylene)malonateHCID 15152794-Amino-3-bromobenzonitrile

生成物 1

HCID 66823182Diethyl 2-((2-bromo-4-cyanophenylamino)methylene)malonate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a solution of 5.00 g (25.4 mmol) 4-amino-3-bromobenzonitrile in 30 mL of toluene was added 8.23 g (38.1 mmol) of diethyl ethoxymethylenemalonate (2a). The mixture was then heated to reflux for overnight with a condenser open to the air. The resulting solution was cooled down to room temperature and poured into 100 mL of hexanes. The white precipitate was collected and washed with hexanes (30 mL×3) to yield 11.9 g of an off-while solid as the desired product. MS ESI (m/z) 367 (M+1)+.

後処理

  1. temperatureThe mixture was then heated
  2. temperatureto reflux for overnight with a condenser open to the air
  3. customThe white precipitate was collected
  4. washwashed with hexanes (30 mL×3)

出典と根拠

ORDレコード
ord-0c863126a77e479c910bf9f517aa3ca5
出典データセット
uspto-grants-2014_04
特許番号
US08697875B2

反応ノート

読み込み中…