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Methyl Acrylate → Methyl (E)-3-(3,5-dichlorophenyl)acrylate

HRID 1480420
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인쇄 미리보기

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HRID 1480420 반응식
[Cl:1][C:2]1[CH:7]=[C:6](I)[CH:5]=[C:4]([Cl:9])[CH:3]=1.[C:10]([O:14][CH3:15])(=[O:13])[CH:11]=[CH2:12].C(N(CC)CC)C>CN(C=O)C.CCOC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6](/[CH:12]=[CH:11]/[C:10]([O:14][CH3:15])=[O:13])[CH:5]=[C:4]([Cl:9])[CH:3]=1
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참가 물질

6

반응물 3

HCID 7294Methyl AcrylateHCID 8471TriethylamineHCID 764241,3-Dichloro-5-iodobenzene

생성물 1

HCID 69907122Methyl (E)-3-(3,5-dichlorophenyl)acrylate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

To 1,3-dichloro-5-iodobenzene (300 mg, 1.099 mmol) and methyl acrylate (0.099 ml, 1.099 mmol) in DMF (10 ml) under nitrogen was added [Pd(t-BuP)]2 (56.1 mg, 0.110 mmol) and triethylamine (0.306 ml, 2.199 mmol). The reaction mixture was heated to 80° C. for 2 h. The reaction mixture was diluted with EtOAc and filtered through a silica cartridge (2 g). The organic solution was washed with water, saturated sodium bicarbonate solution, water and brine. The organic portion was dried using a phase separating column and the solvent was removed under reduced pressure to afford the title compound;

후처리

  1. filtrationfiltered through a silica cartridge (2 g)
  2. washThe organic solution was washed with water, saturated sodium bicarbonate solution, water and brine
  3. customThe organic portion was dried
  4. customseparating column
  5. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-c4cd2e1bef2c4beeb6d60d95b85fd10c
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09409895B2

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