Diethyl 2-((2-bromo-4-cyanophenylamino)methylene)malonate → HCID 178469455、化合物

HRID 2367656ノート

反応式

HRID 2367656 の反応式
[Br:1][C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][C:3]=1[NH:10][CH:11]=[C:12]([C:18]([O:20]CC)=O)[C:13]([O:15][CH2:16][CH3:17])=[O:14]>C1(OC2C=CC=CC=2)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[C:4]2[C:3]=1[N:10]=[CH:11][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:18]2[OH:20]

参加物

3

反応物 1

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

生成物 1

HCID 178469455HCID 178469455、化合物収率 130.3%

試薬・触媒・溶媒 1

HCID 7583Diphenyl Ether溶媒

実験手順

100 mL of diphenyl ether was heated to reflux followed by addition of 5.00 g (13.6 mmol) diethyl 2-((2-bromo-4-cyanophenylamino)methylene)malonate in portions in 30 minutes. The resulting brown solution was reflux for another hour and then cooled down to room temperature. The precipitate was collected and washed with hexanes (15 mL×3) to give 5.69 g of a light brown solid as the desired product. MS ESI (m/z) 321 (M+1)+.

後処理

  1. temperatureto reflux
  2. temperatureThe resulting brown solution was reflux for another hour
  3. customThe precipitate was collected
  4. washwashed with hexanes (15 mL×3)

出典と根拠

ORDレコード
ord-8df4cd917c4c454cbf0df90f444050d8
出典データセット
uspto-grants-2014_04
特許番号
US08697875B2

反応ノート

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