Formic Acid → L-Theanine

HRID 1925774

반응식

HRID 1925774 반응식
CO[C:3]([CH2:5][CH2:6][C@H:7]([NH2:11])[C:8]([OH:10])=[O:9])=[O:4].C(CC(=O)C)(=O)C.[CH2:19]([N:21](CC)CC)[CH3:20].C(N)C.C(O)=O>CO.CC(O)C>[NH2:11][C@H:7]([C:8]([OH:10])=[O:9])[CH2:6][CH2:5][C:3]([NH:21][CH2:19][CH3:20])=[O:4]

참가 물질

8

반응물 5

HCID 284Formic AcidHCID 6341EthylamineHCID 8471TriethylamineHCID 31261AcetylacetoneHCID 686625-Methyl hydrogen L-glutamate

생성물 1

HCID 439378L-Theanine수율 82%

시약·촉매·용매 2

HCID 887Methanol용매HCID 3776Isopropanol용매

반응 조건

온도
60 °C

실험 절차

First, 20.0 g (0.124 mol) of L-glutamic acid-γ-methyl ester was suspended in 20 g of methanol. To this, 13.7 g (0.137 mol) of acetylacetone and 12.5 g (0.124 mol) of triethylamine were added. The mixture was stirred at 60° C. for one hour. Subsequently, 80 g (1.24 mol) of 70% ethylamine was added to the mixture. After the mixture was allowed to react for 6 hours, excessive ethylamine was distilled away under reduced pressure. To this, 11.4 g (0.246 mol) of formic acid and 120 mL of 2-propanol (IPA) were added. The crystal precipitated was filtrated by suction and washed with 20 mL of IPA to obtain wet matter. The wet matter was dried under reduced pressure to obtain 17.7 g of theanine as a white crystal substance (yield: 82%).

후처리

  1. customto react for 6 hours
  2. distillationexcessive ethylamine was distilled away under reduced pressure
  3. customThe crystal precipitated
  4. filtrationwas filtrated by suction
  5. washwashed with 20 mL of IPA
  6. customto obtain wet matter
  7. customThe wet matter was dried under reduced pressure

출처 및 근거

ORD 기록
ord-a804b629c46443cbad14b550f62e952b
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178722B2

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