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Oxalyl chloride → HCID 66749622, 화합물

HRID 537054
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HRID 537054 반응식
[C:1]([NH:4][C:5]1[CH:10]=[C:9]([C:11]2[O:12][C:13]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[Cl:25])=[C:14]([C:16](O)=[O:17])[N:15]=2)[C:8]([CH3:26])=[CH:7][N:6]=1)(=[O:3])[CH3:2].C(Cl)(=O)C(Cl)=O.[CH3:33][O:34][CH:35]([O:38][CH3:39])[CH2:36][NH2:37]>C(Cl)Cl.CN(C=O)C>[C:1]([NH:4][C:5]1[CH:10]=[C:9]([C:11]2[O:12][C:13]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[Cl:25])=[C:14]([C:16]([NH:37][CH2:36][CH:35]([O:38][CH3:39])[O:34][CH3:33])=[O:17])[N:15]=2)[C:8]([CH3:26])=[CH:7][N:6]=1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 65578Oxalyl chlorideHCID 89728Aminoacetaldehyde dimethyl acetalHCID 66749149HCID 66749149, 화합물

생성물 1

HCID 66749622HCID 66749622, 화합물수율 37%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane
용매
3회

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온도
0 °C

실험 절차

A solution of 2-(2-acetamido-5-methylpyridin-4-yl)-5-(2-chlorophenyl)-1,3-oxazole-4-carboxylic acid (0.50 g, 1.34 mmol) in DCM (15 mL) and DMF (0.05 mL) was allowed to stir at 0° C. To this solution was added oxalyl chloride (0.23 mL, 2.69 mmol) dropwise. The reaction mixture was allowed to stir at 0° C. for 15 minutes and then allowed to warm to rt and stir for 2 hr. The reaction mixture was concentrated, and then DCM (15 mL) and TEA (0.38 mL, 2.69 mmol) were added. The reaction mixture was allowed to stir at 0° C. and a solution of 2,2-dimethoxyethanamine (0.29 mL, 2.69 mmol) in DCM (5 mL) was added dropwise. The reaction mixture was allowed to warm to rt and to stir overnight and then concentrated. The residue was redissolved in water and EtOAc. The organic solution was separated and the aqueous solution was further extracted with EtOAc. The organic solutions were combined, dried over MgSO4, filtered and concentrated. The residue was purified by column chromatography to give 2-(2-acetamido-5-methylpyridin-4-yl)-5-(2-chlorophenyl)-N-(2,2-dimethoxyethyl)-1,3-oxazole-4-carboxamide (0.226 g, 37%). LCMS (FA): m/z=459 (M+H).

후처리

  1. stirringto stir at 0° C. for 15 minutes
  2. temperatureto warm to rt
  3. stirringstir for 2 hr
  4. concentrationThe reaction mixture was concentrated
  5. stirringto stir at 0° C.
  6. temperatureto warm to rt
  7. stirringto stir overnight
  8. concentrationconcentrated
  9. dissolutionThe residue was redissolved in water
  10. customThe organic solution was separated
  11. extractionthe aqueous solution was further extracted with EtOAc
  12. dry with materialdried over MgSO4
  13. filtrationfiltered
  14. concentrationconcentrated
  15. customThe residue was purified by column chromatography

출처 및 근거

ORD 기록
ord-048c02e771a34eef9492b8f41b0fe047
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08859768B2

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