Pyridine → HCID 117859737, 화합물

HRID 1486341노트

반응식

HRID 1486341 반응식
[CH3:1][N:2]1[CH:6]=[C:5]([CH:7]([NH2:10])[CH2:8][NH2:9])[CH:4]=[N:3]1.[F:11][C:12]1[CH:33]=[CH:32][CH:31]=[C:30]([F:34])[C:13]=1[CH2:14][O:15][C:16]1[N:21]2[N:22]=[C:23]([CH3:28])[C:24]([C:25](Cl)=[O:26])=[C:20]2[CH:19]=[C:18]([CH3:29])[CH:17]=1.N1C=CC=CC=1>ClC(Cl)C>[NH2:10][CH:7]([C:5]1[CH:4]=[N:3][N:2]([CH3:1])[CH:6]=1)[CH2:8][NH:9][C:25]([C:24]1[C:23]([CH3:28])=[N:22][N:21]2[C:16]([O:15][CH2:14][C:13]3[C:30]([F:34])=[CH:31][CH:32]=[CH:33][C:12]=3[F:11])=[CH:17][C:18]([CH3:29])=[CH:19][C:20]=12)=[O:26]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 435195091154875-76-9HCID 121434555HCID 121434555, 화합물

생성물 1

HCID 117859737HCID 117859737, 화합물

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

14.0 mg (0.10 mmol) of 1-(1-methyl-1H-pyrazol-4-yl)ethane-1,2-diamine were initially charged in a 96-well deep well multititre plate. A solution of 35.1 mg (0.10 mmol) of 7-[(2,6-difluorobenzyl)oxy]-2,5-dimethylpyrazolo[1,5-a]pyridine-3-carbonyl chloride in 0.6 ml of dichloroethane and 0.032 ml (0.40 mmol) of pyridine were added successively and the mixture was stirred at RT overnight. Then the solvent was evaporated off completely, the residue was dissolved in 0.8 ml of DMF and filtered, and the target compound was isolated from the filtrate by preparative LC-MS (Method 9). The product-containing fractions were concentrated under reduced pressure using a centrifugal dryer. The residue of each product fraction was dissolved in 0.6 ml of DMSO. These were combined and finally freed of the solvent in a centrifugal dryer. 18 mg (37% of theory; 94% purity) of the title compound were obtained.

후처리

  1. customThen the solvent was evaporated off completely
  2. dissolutionthe residue was dissolved in 0.8 ml of DMF
  3. filtrationfiltered
  4. customthe target compound was isolated from the filtrate by preparative LC-MS (Method 9)
  5. concentrationThe product-containing fractions were concentrated under reduced pressure
  6. dissolutionThe residue of each product fraction was dissolved in 0.6 ml of DMSO

출처 및 근거

ORD 기록
ord-27522980d049452e8d9b63df25e5c1e0
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422285B2

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