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Sodium Carbonate → HCID 86668047, 화합물

HRID 474076
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HRID 474076 반응식
[Br:1][C:2]1[CH:7]=[C:6]([C:8]2([CH2:15]O)[NH:13][C:12](=[O:14])[CH2:11][O:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1.C([O-])([O-])=O.[Na+].[Na+].C(N(S(F)(F)[F:29])CC)C>C1COCC1>[Br:1][C:2]1[CH:7]=[C:6]([C:8]2([CH2:15][F:29])[NH:13][C:12](=[O:14])[CH2:11][O:10][CH2:9]2)[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium Carbonate2회HCID 123472(Diethylamino)sulfur trifluorideHCID 86668046HCID 86668046, 화합물

생성물 1

HCID 86668047HCID 86668047, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a suspension of 5-(2-bromo-pyridin-4-yl)-5-hydroxymethyl-morpholin-3-one (3.25 g, 11.0 mmol), Na2CO3 (3.5 g, 13.06 mmol) in dry THF (15 ml) was added diethylaminosulfur trifluoride (2.25 ml, 17.0 mmol) at 0° C. The reaction mixture was allowed to warm to rt and stirred for 2 h. Solid Na2CO3 (3.5 g) was again added to the reaction mixture and stirred for 4 h at rt. Solids present in the reaction mixture filtered through Buchner funnel. Filtrate was concentrated under reduced pressure and the crude product was purified by column chromatography using 5% methanol in DCM to obtain title compound as a pale yellow solid.

후처리

  1. stirringstirred for 4 h at rt
  2. filtrationSolids present in the reaction mixture filtered through Buchner funnel
  3. concentrationFiltrate was concentrated under reduced pressure
  4. customthe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-0c42c6db2ccb4d26b23ce4c4e3b3a08c
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637508B2

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