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

HRID 745249노트

반응식

HRID 745249 반응식
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

참가 물질

4

반응물 2

HCID 8857Ethyl AcetateHCID 17517621HCID 17517621, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-66a64d02b43a46558b84213d36509703
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04598077

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