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Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → HCID 57845369, 화합물

HRID 734397
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HRID 734397 반응식
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6](=O)[CH2:5]1)(=[O:3])[CH3:2].C1(P(=[CH:35][C:36]([O:38][CH3:39])=[O:37])(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6]([CH2:35][C:36]([O:38][CH3:39])=[O:37])=[CH:5]1)(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 12477809HCID 12477809, 화합물

생성물 1

HCID 57845369HCID 57845369, 화합물수율 50%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of 1-acetyl-6-methoxy-1,2-dihydro-3H-indol-3-one (3.96 g, 19.3 mmol) (Example 12) and methyl (triphenylphosphoranylidene)acetate (19.75 g, 57.9 mmol) in toluene (60 mL) was heated at reflux under argon for 24 h. The mixture was loaded on silica gel and eluted with EtOAc/hexane (1/5) to yield a thick oil (2.52 g, 50%). LC/MS m/z 262 (M+H)+; 1H NMR (400 MHz, CDCl3) δ 8.04 (br s, 1H), 7.38 (d, 1H), 7.31 (s, 1H), 6.92 (dd, 1H), 3.89 (s, 3H), 3.74 (s, 3H), 3.71 (d, 2H), 2.62 (s, 3H).

후처리

  1. temperaturewas heated
  2. temperatureat reflux under argon for 24 h
  3. washeluted with EtOAc/hexane (1/5)

출처 및 근거

ORD 기록
ord-d34f60c7cd5941d99c34cb677a3c482a
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592361B2

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