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Sodium Chloride → Methyl 5-morpholinopyrazine-2-carboxylate

HRID 639328
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HRID 639328 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[N:9][C:8](Cl)=[CH:7][N:6]=1)=[O:4].[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.CCN(CC)CC.[Na+].[Cl-]>O1CCOCC1.O>[CH3:1][O:2][C:3]([C:5]1[CH:10]=[N:9][C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)=[CH:7][N:6]=1)=[O:4]
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참가 물질

7

반응물 4

HCID 5234Sodium ChlorideHCID 8083MorpholineHCID 8471TriethylamineHCID 406081Methyl 5-chloropyrazine-2-carboxylate

생성물 1

HCID 52987628Methyl 5-morpholinopyrazine-2-carboxylate수율 90.4%

시약·촉매·용매 2

HCID 962Water용매
HCID 31275
1,4-Dioxane
용매

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온도
45 °C

실험 절차

A mixture of 4.9 g (28 mmol) 5-chloro-pyrazine-2-carboxylic acid methyl ester (commercially available), 3.2 g (37 mmol) morpholine and 7.37 g (73 mmol) NEt3 in 50 mL dioxane was heated to 45° C. for 16 h. Water and NaCl aq. was added and the mixture was extracted with ethyl acetate. The combined organic layers were washed with NaCl aq., dried with MgSO4, filtered and evaporated. The residue was recrystallized from ethyl acetate to yield 5.65 g (89%) of the title compound as white solid. m/z (ES+): 224.3 (M+H).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe combined organic layers were washed with NaCl aq.
  3. dry with materialdried with MgSO4
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-c89e6a644aba40e78c1eada2dd145b29
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07691863B2

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