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Diphenyl Ether → HCID 178474057, 화합물

HRID 1170719
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HRID 1170719 반응식
C1(OC2C=CC=CC=2)C=CC=CC=1.[C:14]([NH:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25]([CH3:31])=[CH:26][C:27]([O:29]C)=O)=[CH:20][CH:19]=1)(=[O:16])[CH3:15]>>[OH:29][C:27]1[C:20]2[C:21](=[CH:22][CH:23]=[C:18]([NH:17][C:14](=[O:16])[CH3:15])[CH:19]=2)[N:24]=[C:25]([CH3:31])[CH:26]=1
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참가 물질

3

반응물 2

HCID 7583Diphenyl EtherHCID 284013Methyl 3-{[4-(acetylamino)phenyl]amino}but-2-enoate

생성물 1

HCID 178474057HCID 178474057, 화합물수율 88%

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온도
252.5 °C

실험 절차

Phenyl ether (1 L) was heated to 255° C. Butenoate 3 (334 g, 1.35 mol) was carefully added portionwise while maintaining temperature 245-260° C. After the addition was complete, the yellow-orange suspension was held at 255° C. for an additional 15 min. The mixture was slowly cooled to 40° C., the solids were collected by filtration and washed with EtOAc (3×500 mL) followed by MeOH (3×500 mL) to give hydroxy quinoline 4 as yellow-orange solid (256 g, 88% yield); 1H NMR (DMSO) δ 11.52 (br, s, 1H), 10.07 (s, 1H), 8.24 (s, 1H), 7.82 (d, 1H), 7.42 (d, 1H), 5.84 (s, 1H), 2.31 (s, 3H), 2.05 (s, 1H).

후처리

  1. additionAfter the addition
  2. temperatureThe mixture was slowly cooled to 40° C.
  3. filtrationthe solids were collected by filtration
  4. washwashed with EtOAc (3×500 mL)

출처 및 근거

ORD 기록
ord-8640a03573b147b6b65305e36ac7327c
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07826982B2

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