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Isobutyryl chloride → HCID 86269487, 화합물

HRID 1049346
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HRID 1049346 반응식
[C:1]([NH2:6])(=[O:5])[CH:2]([CH3:4])[CH3:3].C(Cl)(=O)[C:8](Cl)=[O:9].[CH3:13][N:14]1[CH:18]=[C:17]([C:19]2[CH:24]=[C:23]([O:25][C:26]3[CH:27]=[CH:28][C:29]([NH2:36])=[N:30][C:31]=3[C:32]([F:35])([F:34])[F:33])[CH:22]=[CH:21][N:20]=2)[CH:16]=[N:15]1.CCN(C(C)C)C(C)C.C(Cl)(=O)C(C)C>ClCCCl.O1CCOCC1.C(Cl)Cl.[Ag]OC#N.CCOC(C)=O>[CH3:13][N:14]1[CH:18]=[C:17]([C:19]2[CH:24]=[C:23]([O:25][C:26]3[CH:27]=[CH:28][C:29]([NH:36][C:8]([NH:6][C:1](=[O:5])[CH:2]([CH3:4])[CH3:3])=[O:9])=[N:30][C:31]=3[C:32]([F:35])([F:34])[F:33])[CH:22]=[CH:21][N:20]=2)[CH:16]=[N:15]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 62325Isobutyryl chlorideHCID 65578Oxalyl chloride2회HCID 68424Isobutyramide2회HCID 81531DiisopropylethylamineHCID 90403125HCID 90403125, 화합물

생성물 1

HCID 86269487HCID 86269487, 화합물수율 45%

시약·촉매·용매 5

HCID 178513473HCID 178513473, 화합물촉매HCID 111,2-Dichloroethane용매3회HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

실험 절차

A suspension of Example B7 (0.021 g, 0.246 mmol) in DCE (3 mL) was treated with oxalyl chloride (0.022 mL, 0.246 mmol), stirred at RT for 5 min, then heated at 80° C. for 1 h. The mixture was cooled to RT, added drop-wise to a solution of 5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)-6-(trifluoromethyl)pyridin-2-amine (0.055 g, 0.164 mmol) and DIEA (0.172 mL, 0.984 mmol) in dioxane (3 mL) and stirred at RT overnight. A solution of silver cyanate (0.246 g, 1.640 mmol) in DCM (3 mL) was treated with isobutyryl chloride (0.035 g, 0.328 mmol), stirred at RT for 2 h, then added to the DCE mixture and stirred at RT for 2 h. A second suspension of Example B7 (140 mg) in DCE (4 mL) was treated with oxalyl chloride (0.15 mL), heated at 80° C. for 2 h, cooled to RT, added to the original reaction mixture and stirred at RT overnight. The mixture was treated with EtOAc and the solids removed via filtration through diatomaceous earth. The filtrate was washed with satd. NaHCO3 (2×) and the combined organics were dried over Na2SO4, concentrated to dryness and purified via silica gel chromatography (MeOH/EtOAc) to afford N-((5-((2-(1-methyl-1H-pyrazol-4-yl)pyridin-4-yl)oxy)-6-(trifluoromethyl)pyridin-2-yl)carbamoyl)isobutyramide (33 mg, 45%) as a light brown solid. 1H NMR (400 MHz, DMSO-d6): δ 11.28 (s, 1H), 10.97 (s, 1H), 8.40 (d, J=5.7 Hz, 1H), 8.34 (d, J=9.1 Hz, 1H), 8.28 (s, 1H), 7.98-7.97 (m, 2H), 7.29 (d, J=2.5 Hz, 1H), 6.78 (dd, J=5.7, 2.5 Hz, 1H), 3.84 (s, 3H), 2.72-2.63 (m, 1H), 1.10 (d, J=6.8 Hz, 6H); MS (ESI) m/z: 449.2 (M+H+).

후처리

  1. temperatureheated at 80° C. for 1 h
  2. temperatureThe mixture was cooled to RT
  3. stirringstirred at RT overnight
  4. stirringstirred at RT for 2 h
  5. stirringstirred at RT for 2 h
  6. temperatureheated at 80° C. for 2 h
  7. temperaturecooled to RT
  8. additionadded to the original reaction mixture
  9. stirringstirred at RT overnight
  10. customthe solids removed via filtration through diatomaceous earth
  11. washThe filtrate was washed with satd
  12. dry with materialNaHCO3 (2×) and the combined organics were dried over Na2SO4
  13. concentrationconcentrated to dryness
  14. custompurified via silica gel chromatography (MeOH/EtOAc)

출처 및 근거

ORD 기록
ord-0c712016d6a2414a8babe304b5f4f733
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382228B2

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