Diphenyl Ether → HCID 178469490, 화합물

HRID 1042977노트

반응식

HRID 1042977 반응식
[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

참가 물질

3

반응물 2

HCID 7583Diphenyl EtherHCID 57465569Diethyl ({[3-(3,5-dimethyl-4-isoxazolyl)phenyl]amino}methylidene)-propanedioate2회

생성물 1

HCID 178469490HCID 178469490, 화합물수율 76%

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-18c3f4fda8cb4893bc83b38453c9b540
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557984B2

반응 노트

불러오는 중…