3-Amino-3-(4-nitrophenyl)-2-cyanoacrylonitrile → HCID 59099563、化合物

HRID 227616

反応式

HRID 227616 の反応式
[NH2:1][C:2]([C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[C:3]([C:6]#[N:7])[C:4]#[N:5].P([O-])(OCC)(SCC)=[S:18]>C(O)C.O>[NH2:1]/[C:2](/[C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1)=[C:3](/[C:4]#[N:5])\[C:6](=[S:18])[NH2:7]

参加物

5

反応物 2

HCID 140279223-Amino-3-(4-nitrophenyl)-2-cyanoacrylonitrileHCID 53249491Diethyldithiophosphate

生成物 1

HCID 59099563HCID 59099563、化合物収率 95%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A suspension of Example 96C (2.1 g, 9.8 mmol) and 90% diethyl dithiophosphate (1.8 mL, 10.8 mmol) in ethanol (15 mL) and water (15 mL) was heated to reflux for 24 hours, cooled to room temperature, poured into ice water (300 mL), and filtered. The filter cake was dried to provide 2.3 g (95% yield) of the desired product. MS(ESI(−)) m/e 247 (M−H)−.

後処理

  1. temperatureto reflux for 24 hours
  2. filtrationfiltered
  3. customThe filter cake was dried

出典と根拠

ORDレコード
ord-631e3ab4d3404d2c9f8160fcdda6472d
出典データセット
uspto-grants-2009_07
特許番号
US07560552B2

関連ノート

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