Beta-Alanine → 3-(Cyclohexylformamido)propanoic acid

HRID 1428419노트

반응식

HRID 1428419 반응식
[NH2:1][CH2:2][CH2:3][C:4]([OH:6])=[O:5].[OH-].[Na+].[CH:9]1([C:15](Cl)=[O:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1.Cl>O>[CH:9]1([C:15]([NH:1][CH2:2][CH2:3][C:4]([OH:6])=[O:5])=[O:16])[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

참가 물질

6

반응물 4

HCID 239Beta-AlanineHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 75938Cyclohexanecarbonyl chloride

생성물 1

HCID 119834713-(Cyclohexylformamido)propanoic acid수율 85%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Ten grams of β-alanine and 9 g of sodium hydroxide were dissolved in 100 mL of purified water, and 14.9 g of cyclohexanecarbonyl chloride were added dropwise under freezing conditions. After stirring for five hours, hydrochloric acid was added and the pH was adjusted to 2 or less. After extraction with 500 mL of ethyl acetate, the product was desiccated over magnesium sulfate, filtered, and concentrated under reduced pressure. The resulting residue was recrystallized with aqueous ethanol, and 17.2 g of the desired product was obtained (yield of 85%).

후처리

  1. extractionAfter extraction with 500 mL of ethyl acetate
  2. filtrationfiltered
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was recrystallized with aqueous ethanol

출처 및 근거

ORD 기록
ord-7123eef2ed094a5e80f4dfc4d6e1b5a9
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937090B2

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