Methanol → Diethyl 2-acetamido-2-(2-pentadecynyl)malonate

HRID 862829노트

반응식

HRID 862829 반응식
[C:1]([NH:4][CH:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])(=[O:3])[CH3:2].[CH3:16][CH2:17][O-].[Na+].[CH2:20]([C:28]1[CH:33]=[CH:32][C:31](CCO)=[CH:30][CH:29]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]C.CO>C(O)C>[C:1]([NH:4][C:5]([CH2:26][C:25]#[C:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:17][CH3:16])([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])(=[O:3])[CH3:2]

참가 물질

6

반응물 4

HCID 887MethanolHCID 14041Acetamidomalonic acid diethyl esterHCID 2723922Sodium ethoxideHCID 113108762-(4-Octylphenyl)ethanol

생성물 1

HCID 21849278Diethyl 2-acetamido-2-(2-pentadecynyl)malonate

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

Diethyl acetamidomalonate (3.327 g) and 1.137 g of sodium ethylate were dissolved in 50 ml of dry ethanol and the mixture was stirred at room temperature for 30 minutes under a nitrogen atmosphere. A solution of 4.000 g of the compound of (3) above in 30 ml of dry ethanol was added thereto and the mixture was refluxed for 15 hours. Methanol (50 ml) was added to the reaction mixture and the insoluble matters were removed. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography to give 3.236 g of diethyl 2-acetamido-2-(2-pentadecynyl)malonate.

후처리

  1. temperaturethe mixture was refluxed for 15 hours
  2. customthe insoluble matters were removed
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-d6deb23ebbca4508ab88028d7aea6871
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05719176

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