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

HRID 1480420
ノート
印刷プレビュー

反応式

HRID 1480420 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

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;

後処理

  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

出典と根拠

ORDレコード
ord-c4cd2e1bef2c4beeb6d60d95b85fd10c
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09409895B2

反応ノート

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