Ethyl Acetate → Methyl beta-phthalimido-beta-(4-methylphenyl)propionate

HRID 745249ノート

反応式

HRID 745249 の反応式
Cl.[NH2:2][CH:3]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)[CH2:4][C:5]([O:7][CH3:8])=[O:6].C([O:19][CH2:20][CH3:21])(=O)C>C(N(CC)CC)C>[C:20]1(=[O:19])[N:2]([CH:3]([C:9]2[CH:10]=[CH:11][C:12]([CH3:15])=[CH:13][CH:14]=2)[CH2:4][C:5]([O:7][CH3:8])=[O:6])[C:5](=[O:6])[C:4]2=[CH:3][CH:9]=[CH:10][CH:11]=[C:21]12

参加物

4

反応物 2

HCID 8857Ethyl AcetateHCID 17517621HCID 17517621、化合物

生成物 1

HCID 13655327Methyl beta-phthalimido-beta-(4-methylphenyl)propionate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To 14 g of methyl β-amino-β-(4-methylphenyl)propionate hydrochloride, were added 200 ml of ethyl acetate and 10.2 ml of triethylamine. The mixture was stirred at room temperature for 30 minutes, then washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was evaporated under reduced pressure. To the residue, was added 8.5 g of phthalic anhydride. The mixture was stirred at 150° to 155° C. for one hour and recrystallized from an ether-n-hexane mixture to yield 15 g of methyl β-phthalimido-β-(4-methylphenyl)propionate; m.p. 97°-99° C.

後処理

  1. washwashed with saturated aqueous sodium chloride solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customThe filtrate was evaporated under reduced pressure
  5. additionTo the residue, was added 8.5 g of phthalic anhydride
  6. stirringThe mixture was stirred at 150° to 155° C. for one hour
  7. customrecrystallized from an ether-n-hexane mixture

出典と根拠

ORDレコード
ord-66a64d02b43a46558b84213d36509703
出典データセット
uspto-grants-1986_07
特許番号
US04598077

反応ノート

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