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

HRID 70104노트

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HRID 70104 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-40089829728845ff8fc14aa42052cb59
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822474B2

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