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Diethyl Ether → HCID 58307292, 화합물

HRID 448321
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HRID 448321 반응식
[CH3:1][O:2][C:3](=[O:15])[C:4]1[C:5](=[C:10](Br)[CH:11]=[CH:12][CH:13]=1)[C:6]([O:8][CH3:9])=[O:7].C([O-])([O-])=O.[Cs+].[Cs+].[CH3:22][O:23][CH2:24][CH:25]([NH2:27])[CH3:26].C(OCC)C>C1(C)C=CC=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH3:1][O:2][C:3](=[O:15])[C:4]1[C:5](=[C:10]([NH:27][CH:25]([CH3:26])[CH2:24][O:23][CH3:22])[CH:11]=[CH:12][CH:13]=1)[C:6]([O:8][CH3:9])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 10796Cesium carbonateHCID 123458MethoxyisopropylamineHCID 53438518Dimethyl 3-bromophthalate

생성물 1

HCID 58307292HCID 58307292, 화합물수율 38%

시약·촉매·용매 2

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매

실험 절차

To a stirred solution of 3-Bromophthalic acid dimethyl ester (0.82 g, 3.0 mmol) in toluene (20 mL), were added S-BINAP (56 mg, 0.09 mmol), Pd2(dba)3 (55 mg, 0.06 mmol), Cs2CO3 (1.37 g, 4.2 mmol), and 1-methoxy-2-propanamine (0.32 g, 3.6 mmol), and the resulting mixture was heated to reflux with stirring under nitrogen for 24 hours. The mixture was allowed to cool to room temperature, and diethyl ether was added (70 mL). The mixture was filtered, and the filtrate was evaporated in vacuo. The residue was chromatographed eluting with 17:3 hexanes-ethyl acetate. The resulting material was further purified by preparative HPLC, eluting with 11:9 water-acetonitrile, and providing 0.32 g of the product in 38% yield: 1H NMR (DMSO-d6) δ1.14 (d, J=6.4 Hz, 3H), 3.29 (s, 3H), 3.37 (d, J=4.8 Hz, 2H), 3.74 (s, 3H), 3.77 (s, 3H), 3.74-3.80 (m, 1H), 6.53 (d, J=7.8 Hz, 1H), 6.76 (d, J=7.3 Hz, 1H), 6.99 (d, J=8.6 Hz, 1H), 7.38 (t, J=7.8 Hz, 1H).

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux
  3. filtrationThe mixture was filtered
  4. customthe filtrate was evaporated in vacuo
  5. customThe residue was chromatographed
  6. washeluting with 17:3 hexanes-ethyl acetate
  7. customThe resulting material was further purified by preparative HPLC
  8. washeluting with 11:9 water-acetonitrile

출처 및 근거

ORD 기록
ord-870a0029f3b84030b8f2cd1b9c5679f8
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481568B2

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