Water → methyl(Z)-4-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-3-methoxy-but-2-enoate

HRID 70104ノート

反応式

HRID 70104 の反応式
[C:1]1(=[O:11])[NH:5][C:4](=[O:6])[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[K].Cl[CH2:14][C:15]([O:21][CH3:22])=[CH:16][C:17]([O:19][CH3:20])=[O:18].O>CN(C=O)C>[O:6]=[C:4]1[C:3]2[C:2](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:1](=[O:11])[N:5]1[CH2:14]/[C:15](/[O:21][CH3:22])=[CH:16]/[C:17]([O:19][CH3:20])=[O:18]

参加物

5

反応物 3

HCID 962WaterHCID 5838182-Butenoic acid, 4-chloro-3-methoxy-, methyl esterHCID 24194345Phthalimide potassium salt

生成物 1

HCID 59708416methyl(Z)-4-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-3-methoxy-but-2-enoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
60 °C

実験手順

18.5 potassium phthalimide are suspended in 50 ml DMF, the mixture is heated to 60° C. and 16.5 g methyl 4-chloro-3-methoxy-but-2-enoate in 50 ml DMF are added. After 2 days the reaction mixture is poured into 500 ml of water. The precipitate formed is suction filtered and washed with water. The residue is dissolved in ethyl acetate, dried and the solution is evaporated to dryness. The residue is triturated with ether. 21.77 g of the product are obtained as a powder.

後処理

  1. customThe precipitate formed
  2. filtrationfiltered
  3. washwashed with water
  4. dissolutionThe residue is dissolved in ethyl acetate
  5. customdried
  6. customthe solution is evaporated to dryness
  7. customThe residue is triturated with ether

出典と根拠

ORDレコード
ord-40089829728845ff8fc14aa42052cb59
出典データセット
uspto-grants-2014_09
特許番号
US08822474B2

反応ノート

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