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Triethylamine → HCID 57384340, 화합물

HRID 706671
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HRID 706671 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][N:9]2[C:12]([C:15]([OH:17])=O)=[CH:13][N:14]=[C:8]2[CH:7]=1.C(N(CC)CC)C.ClC1C=C(Cl)C=C(Cl)C=1C(Cl)=O.[NH2:37][C:38]1[CH:46]=[CH:45][CH:44]=[C:43]2[C:39]=1[CH:40]=[N:41][N:42]2[CH2:47][C:48]1[CH:49]=[C:50]([CH:55]=[CH:56][CH:57]=1)[C:51]([O:53][CH3:54])=[O:52]>CCOC(C)=O.CN1C(=O)CCC1>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]1[CH:11]=[CH:10][N:9]2[C:12]([C:15]([NH:37][C:38]3[CH:46]=[CH:45][CH:44]=[C:43]4[C:39]=3[CH:40]=[N:41][N:42]4[CH2:47][C:48]3[CH:49]=[C:50]([CH:55]=[CH:56][CH:57]=3)[C:51]([O:53][CH3:54])=[O:52])=[O:17])=[CH:13][N:14]=[C:8]2[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 27337032,4,6-Trichlorobenzoyl chlorideHCID 667820257-(2-Methoxyethoxy)imidazo[1,2-a]pyridine-3-carboxylic acidHCID 67976218HCID 67976218, 화합물

생성물 1

HCID 57384340HCID 57384340, 화합물수율 80.1%

시약·촉매·용매 2

HCID 8857
Ethyl Acetate
용매
HCID 13387N-methyl-2-pyrrolidone용매2회

반응 조건

온도
80 °C

실험 절차

To a vial was added 7-(2-methoxyethoxy)imidazo[1,2-a]pyridine-3-carboxylic acid (0.260 g, 1.05 mmol) and NMP (3.5 mL). Triethylamine (0.243 mL, 1.74 mmol) was added and the mixture was stirred until homogeneous. 2,4,6-Trichlorobenzoyl chloride (0.153 mL, 0.975 mmol) was added and the mixture was stirred at ambient temperature for 0.5 hours. Methyl 3-((4-amino-1H-indazol-1-yl)methyl)benzoate (0.196 g, 0.697 mmol) was added as a NMP solution (1.2 mL), and the reaction mixture was sealed in the vial and warmed to 80° C. with stirring overnight. The reaction mixture was cooled and diluted with EtOAc (20 mL), and then filtered to remove white solids. The solids were washed with EtOAc and the filtrate was concentrated under vacuum until only DMA was left. The concentrated solution diluted with water/saturated aqueous NaHCO3 (25 mL, 1:1) forming a precipitate. The precipitate was isolated by filtration and the solid was washed with water, Et2O, and hexanes, then dried under vacuum at 40° C. for 4 hours to provide 0.279 g (74%) of the title compound. MS (ES+APCI) m/z=500 (M+H).

후처리

  1. stirringthe mixture was stirred at ambient temperature for 0.5 hours
  2. customthe reaction mixture was sealed in the vial and
  3. stirringwith stirring overnight
  4. temperatureThe reaction mixture was cooled
  5. filtrationfiltered
  6. customto remove white solids
  7. washThe solids were washed with EtOAc
  8. concentrationthe filtrate was concentrated under vacuum until only DMA
  9. waitwas left
  10. additionThe concentrated solution diluted with water/saturated aqueous NaHCO3 (25 mL, 1:1)
  11. customforming a precipitate
  12. customThe precipitate was isolated by filtration
  13. washthe solid was washed with water, Et2O, and hexanes
  14. customdried under vacuum at 40° C. for 4 hours

출처 및 근거

ORD 기록
ord-e96945e693714ef0bd200c7b0fdaca33
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174981B2

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