Diphenyl Ether → HCID 178469490、化合物

HRID 1042977ノート

反応式

HRID 1042977 の反応式
[CH3:1][C:2]1[C:6]([C:7]2[CH:8]=[C:9]([NH:13][CH:14]=[C:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[C:16](OCC)=[O:17])[CH:10]=[CH:11][CH:12]=2)=[C:5]([CH3:26])[O:4][N:3]=1.C1(OC2C=CC=CC=2)C=CC=CC=1>>[CH3:1][C:2]1[C:6]([C:7]2[CH:8]=[C:9]3[C:10]([C:16]([OH:17])=[C:15]([C:21]([O:23][CH2:24][CH3:25])=[O:22])[CH:14]=[N:13]3)=[CH:11][CH:12]=2)=[C:5]([CH3:26])[O:4][N:3]=1

参加物

3

反応物 2

HCID 7583Diphenyl EtherHCID 57465569Diethyl ({[3-(3,5-dimethyl-4-isoxazolyl)phenyl]amino}methylidene)-propanedioate2 回

生成物 1

HCID 178469490HCID 178469490、化合物収率 76%

実験手順

Diethyl ({[3-(3,5-dimethyl-4-isoxazolyl)phenyl]amino}methylidene)-propanedioate (for a preparation see Intermediate 5, 75 g, 210 mmol) was suspended in boiling diphenylether (1 L) and heated to reflux for 30 minutes. The reaction mixture was cooled and precipitated with iPr2O to give the title compound as a brown powder (50 g, 76%). 1H NMR (300 MHz, DMSO-d6, ppm) δ: 12.45 (brs, 1H), 8.76 (s, 1H), 8.34 (d, J=8.6 Hz, 1H), 7.76 (s, 1H), 7.59 (d, J=8.6 Hz, 1H), 4.36 (q, J=7.1 Hz, 2H), 2.62 (s, 3H), 2.43 (s, 3H), 1.43 (s, J=7.1 Hz, 3H).

後処理

  1. temperatureheated
  2. temperatureto reflux for 30 minutes
  3. temperatureThe reaction mixture was cooled
  4. customprecipitated with iPr2O

出典と根拠

ORDレコード
ord-18c3f4fda8cb4893bc83b38453c9b540
出典データセット
uspto-grants-2013_10
特許番号
US08557984B2

反応ノート

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