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Cesium carbonate → 3-[4-(2-Dimethylamino-ethoxy)-2-isopropoxy-phenylamino]-phthalic acid dimethyl ester

HRID 448382
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HRID 448382 반응식
[CH3:1][O:2][C:3](=[O:15])[C:4]1[C:5](=[C:10](I)[CH:11]=[CH:12][CH:13]=1)[C:6]([O:8][CH3:9])=[O:7].[CH3:16][N:17]([CH3:32])[CH2:18][CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([NH2:27])=[C:23]([O:28][CH:29]([CH3:31])[CH3:30])[CH:22]=1.C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.C(=O)([O-])[O-].[Cs+].[Cs+]>C1(C)C=CC=CC=1.C(Cl)Cl.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][C:24]2[CH:25]=[CH:26][C:21]([O:20][CH2:19][CH2:18][N:17]([CH3:32])[CH3:16])=[CH:22][C:23]=2[O:28][CH:29]([CH3:31])[CH3:30])[CH:11]=[CH:12][CH:13]=1)[C:6]([O:8][CH3:9])=[O:7]
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참가 물질

8

반응물 4

HCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 2326127Dimethyl 3-iodophthalateHCID 583071884-(2-Dimethylaminoethoxy)-2-isopropoxyphenylamine

생성물 1

HCID 583073113-[4-(2-Dimethylamino-ethoxy)-2-isopropoxy-phenylamino]-phthalic acid dimethyl ester수율 47%

시약·촉매·용매 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 1140Toluene용매
HCID 6344Dichloromethane용매

실험 절차

A mixture of 3-iodophthalic acid dimethyl ester (2.0 g, 6.2 mmol), 4-(2-dimethylaminoethoxy)-2-isopropoxyphenylamine (1.5 g, 6.2 mmol), Pd2(dba)3 (0.26 g, 0.28 mmol), rac-BINAP (0.12 g, 0.19 mmol), and cesium carbonate (2.8 g, 8.6 mmol), in 12 mL toluene was heated to reflux under nitrogen for 24 hours. The reaction mixture was cooled, diluted with CH2Cl2 (20 mL), and filtered through Celite, and the filter was washed with additional CH2Cl2 (60 mL). The filtrate was evaporated in vacuo, and the residue was purified by ISCO silica gel flash chromatography using a methylene chloride-methanol gradient, eluting 1.3 g of the product at 96:4 methylene chloride-methanol, in 47% yield; 1H NMR (CDCl3) δ 1.31 (d, J=6.1 Hz, 6H), 2.96 (d, J=4.8 Hz, 6H), 3.41-3.47 (m, 2H), 3.87 (s, 6H), 4.47-4.51 (m, 3H), 6.45 (dd, J=8.7 Hz, J=2.6 Hz, 1H), 6.56 (d, J=2.6 Hz, 1H), 7.07 (dd, J=6.0 Hz, J=2.5 Hz, 1H), 7.18 (d, J=8.7 Hz, 1H), 7.20-7.18 (m, 2H), 7.90 (s, 1H).

후처리

  1. temperatureto reflux under nitrogen for 24 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered through Celite
  4. washthe filter was washed with additional CH2Cl2 (60 mL)
  5. customThe filtrate was evaporated in vacuo
  6. customthe residue was purified by ISCO silica gel flash chromatography
  7. washeluting 1.3 g of the product at 96:4 methylene chloride-methanol

출처 및 근거

ORD 기록
ord-f0485f090fdb41a5b6e4126d0d0ae622
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481568B2

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