Hydrochloric Acid → HCID 178487705, 화합물

HRID 1188735노트

반응식

HRID 1188735 반응식
[Cl:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:12](O)=[O:13])[CH:8]=[C:7]2[OH:15].[CH3:18][NH:19][CH3:20].C1COCC1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN1CCOCC1.Cl>CN(C=O)C.CCOC(C)=O>[CH3:18][N:19]([CH3:20])[C:12]([C:9]1[CH:8]=[C:7]([OH:15])[C:6]2[C:11](=[C:2]([Cl:1])[C:3]([O:16][CH3:17])=[CH:4][CH:5]=2)[N:10]=1)=[O:13]

참가 물질

9

반응물 6

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 79724-MethylmorpholineHCID 8028TetrahydrofuranHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178487707HCID 178487707, 화합물

생성물 1

HCID 178487705HCID 178487705, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

The 8-chloro-4-hydroxy-7-methoxy-quinoline-2-carboxylic acid (500 mg, 1.97 mmol) and 2.0 M dimethylamine in THF (2 mL, 3.94 mmol) were dissolved in DMF (20 mL). HATU (1.5 g, 3.94 mmol) and NMM (697 mg, 6.89 mmol) were added and the mixture was stirred at r.t. overnight. The reaction was diluted with EtOAc and acidified with 1 N HCl. The two layers were separated. The organic layer was washed with 2% LiCl, saturated NaHCO3 and brine, dried with Na2SO4, and concentrated to give 8-chloro-4-hydroxy-7-methoxy-quinoline-2-carboxylic acid dimethylamide.

후처리

  1. customThe two layers were separated
  2. washThe organic layer was washed with 2% LiCl, saturated NaHCO3 and brine
  3. dry with materialdried with Na2SO4
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ac172748bba94e6293dcf87b1b360fd6
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674088B2

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