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Thionyl Chloride → HCID 57749087, 화합물

HRID 1874462
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HRID 1874462 반응식
[CH3:1][C:2]1[S:3][C:4]([CH3:10])=[C:5]([C:7]([OH:9])=O)[N:6]=1.S(Cl)(Cl)=O.[NH2:15][C:16]1[CH:17]=[C:18]([CH:35]=[CH:36][C:37]=1[CH3:38])[O:19][C:20]1[CH:21]=[CH:22][C:23]2[N:24]([N:26]=[C:27]([NH:29][C:30]([CH:32]3[CH2:34][CH2:33]3)=[O:31])[N:28]=2)[CH:25]=1>O1CCCC1.CN(C)C=O.C(=O)([O-])O.[Na+]>[CH:32]1([C:30]([NH:29][C:27]2[N:28]=[C:23]3[CH:22]=[CH:21][C:20]([O:19][C:18]4[CH:35]=[CH:36][C:37]([CH3:38])=[C:16]([NH:15][C:7]([C:5]5[N:6]=[C:2]([CH3:1])[S:3][C:4]=5[CH3:10])=[O:9])[CH:17]=4)=[CH:25][N:24]3[N:26]=2)=[O:31])[CH2:33][CH2:34]1
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참가 물질

7

반응물 3

HCID 24386Thionyl ChlorideHCID 13835313Dimethyl-1,3-thiazole-4-carboxylic acidHCID 57749401N-[6-(3-amino-4-methylphenoxy)[1,2,4]triazolo[1,5-a]pyridin-2-yl]cyclopropanecarboxamide

생성물 1

HCID 57749087HCID 57749087, 화합물수율 87%

시약·촉매·용매 3

HCID 6228Dimethylformamide촉매
HCID 8028
Tetrahydrofuran
용매
HCID 516892Sodium Bicarbonate용매

실험 절차

To a solution of 2,5-dimethyl-1,3-thiazole-4-carboxylic acid (107 mg, 0.681 mmol) in tetrahydrofuran (5 mL) were added N,N-dimethylformamide (2 drops) and thionyl chloride (118 μL, 1.36 mmol), and the mixture was stirred at room temperature for 2 hr. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in N,N-dimethylacetamide (6 mL). N-[6-(3-Amino-4-methylphenoxy)[1,2,4]triazolo[1,5-a]pyridin-2-yl]cyclopropanecarboxamide (200 mg, 0.619 mmol) was added thereto, and the mixture was stirred at room temperature for 2 hr. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate and filtrated. The filtrate was concentrated under reduced pressure, the residue was and recrystallized from ethanol to give the title compound (248 mg, 87%) as a white solid.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in N,N-dimethylacetamide (6 mL)
  3. stirringthe mixture was stirred at room temperature for 2 hr
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltrated
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-179121824d484c51937247734b852708
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08304557B2

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