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Hydrochloric Acid → HCID 178499132, 화합물

HRID 869728
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HRID 869728 반응식
C(OC([NH:8][C@H:9]([C:11]([NH:13][C@@H:14]([C:19](=O)[CH3:20])[C:15]([O:17][CH3:18])=[O:16])=[O:12])[CH3:10])=O)(C)(C)C.Cl>O1CCOCC1>[OH:12][C:11]1[N:13]=[C:14]([C:15]([O:17][CH3:18])=[O:16])[C:19]([CH3:20])=[N:8][C:9]=1[CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

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HCID 313Hydrochloric AcidHCID 86674523methyl (2S)-2-{[N-(tert-butoxycarbonyl)-L-alanyl]amino}-3-oxobutanoate

생성물 1

HCID 178499132HCID 178499132, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

A solution of methyl (2S)-2-{[N-(tert-butoxycarbonyl)-L-alanyl]amino}-3-oxobutanoate (3.05 g, 10.1 mmol) and 4N hydrochloric acid in 1,4-dioxane (10 mL) was stirred at room temperature. After being stirred for 1 h at same temperature, the reaction mixture was concentrated in vacuo. A solution of the residue in pyridine (50 mL) was heated at 60° C. for 4 h. After being cooled to ambient temperature, the mixture was concentrated in vacuo. The residue was poured into water, and the mixture was extracted with dichloromethane. The organic layer was washed with saturated brine, dried over magnesium sulfate, filtrated and concentrated in vacuo. The residue was triturated with hexane-ethyl acetate (1:1) to give methyl 6-hydroxy-3,5-dimethylpyrazine-2-carboxylate. MS (APCI): m/z 183 (M+H).

후처리

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. temperatureAfter being cooled to ambient temperature
  3. concentrationthe mixture was concentrated in vacuo
  4. additionThe residue was poured into water
  5. extractionthe mixture was extracted with dichloromethane
  6. washThe organic layer was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltrated
  9. concentrationconcentrated in vacuo
  10. customThe residue was triturated with hexane-ethyl acetate (1:1)

출처 및 근거

ORD 기록
ord-08c8b399f72e42feab2cd18ef302586f
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969376B2

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