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Potassium Hydroxide → HCID 17851043, 화합물

HRID 1374995
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HRID 1374995 반응식
C([O:3][C:4](=[O:25])[C:5]([NH:21][C:22](=[O:24])[CH3:23])([CH2:11][C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([O:19][CH3:20])[CH:13]=1)C(OCC)=O)C.[OH-].[K+]>O.C(O)C>[C:22]([NH:21][CH:5]([C:4]([OH:25])=[O:3])[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[C:14]([O:19][CH3:20])[CH:13]=1)(=[O:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14797Potassium Hydroxide2회HCID 13406780HCID 13406780, 화합물

생성물 1

HCID 17851043HCID 17851043, 화합물수율 106%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

A mixture of 2-acetylamino-2-(3-methoxy-4-methylbenzyl)-malonic acid diethyl ester (10.0 g), potassium hydroxide solution (1.88 g) in water (25 ml) and ethanol (25 ml) were stirred under reflux for 1 hour. Another potassium hydroxide solution (1.88 g) in water (10 ml) was added to the mixture and the whole was stirred under reflux for 2 hours. After being cooled to room temperature, the reaction mixture was concentrated under reduced pressure. Water (50 ml) and ethyl acetate (50 ml) were added to the resulting aqueous solution. The aqueous layer was separated and was adjusted to pH 1.5 with 6N hydrochloric acid. The solution was extracted with ethyl acetate, washed with brine, dried over sodium sulfate and evaporated under reduced pressure to give N-acetyl-3-methoxy-4-methyl-DL-phenylalanine (7.58 g) as a viscous oil.

후처리

  1. temperatureunder reflux for 1 hour
  2. stirringthe whole was stirred
  3. temperatureunder reflux for 2 hours
  4. concentrationthe reaction mixture was concentrated under reduced pressure
  5. additionWater (50 ml) and ethyl acetate (50 ml) were added to the resulting aqueous solution
  6. customThe aqueous layer was separated
  7. extractionThe solution was extracted with ethyl acetate
  8. washwashed with brine
  9. dry with materialdried over sodium sulfate
  10. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-40d21ff615ce438b82d43c5d9337f3cc
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166598B2

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