L-Phenylalanine → HCID 66739398, 화합물

HRID 2066343노트

반응식

HRID 2066343 반응식
[NH2:1][C@H:2]([C:10]([OH:12])=[O:11])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH2:13](O)[CH2:14][CH2:15]CCCCCCCCC>S(=O)(=O)(O)O.O.C1(C)C=CC=CC=1>[C:10]([OH:12])(=[O:11])[CH2:2][CH2:3][CH2:4][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:13][CH2:14][CH3:15].[NH2:1][C@H:2]([C:10]([OH:12])=[O:11])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

6

반응물 2

HCID 6140L-PhenylalanineHCID 81931-Dodecanol

생성물 1

HCID 66739398HCID 66739398, 화합물

시약·촉매·용매 3

HCID 962Water용매2회HCID 1118Sulfuric Acid용매HCID 1140Toluene용매

실험 절차

16.52 g of phenylalanine was dissolved in a solution of 10 g of concentrated sulfuric acid, 20 mL water, 20 mL of dodecanol, and 120 mL of toluene in a 500 mL round bottom flask equipped with a condenser and a Dean-Stark apparatus. The resulting solution was heated at reflux temperature until no more water could be distilled. The resulting solution was then cooled to room temperature and washed with saturated aqueous sodium bicarbonate to neutralize acidic impurities, washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was then removed under reduced pressure to provide phenylalanine dodecanoate as a solid that was purified using a silica gel column eluted with a 1:9 methanol:dichloromethane mixture.

후처리

  1. customequipped with a condenser
  2. temperatureThe resulting solution was heated
  3. distillationcould be distilled
  4. washwashed with saturated aqueous sodium bicarbonate
  5. washwashed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was then removed under reduced pressure

출처 및 근거

ORD 기록
ord-e20c26db6c0a4307be6f1da5a825879f
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293253B2

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