Potassium Phosphate, Tribasic → HCID 66807421, 화합물

HRID 1843979

반응식

HRID 1843979 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:13][C:12]3[CH2:11][CH2:10][NH:9][C:8](=[O:14])[C:7]=3[C:6]=2[CH:15]=1.Br[C:17]1[CH:18]=[N:19][CH:20]=[CH:21][C:22]=1[C:23]([F:26])([F:25])[F:24].P([O-])([O-])([O-])=O.[K+].[K+].[K+]>[Cu](I)I.O1CCOCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:13][C:12]3[CH2:11][CH2:10][N:9]([C:17]4[CH:18]=[N:19][CH:20]=[CH:21][C:22]=4[C:23]([F:26])([F:25])[F:24])[C:8](=[O:14])[C:7]=3[C:6]=2[CH:15]=1

참가 물질

6

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 199372633-Bromo-4-(trifluoromethyl)pyridineHCID 89964175HCID 89964175, 화합물

생성물 1

HCID 66807421HCID 66807421, 화합물수율 9.1%

시약·촉매·용매 2

HCID 83717Copper iodide촉매HCID 312751,4-Dioxane용매

실험 절차

Using analogous conditions and workup as described for the preparation of Example 1A above, 8-fluoro-3,4-dihydro-2H-benzo[4,5]thieno[3,2-c]pyridin-1-one (I-50g: 100 mg, 0.452 mmol) was reacted with 3-bromo-4-trifluoromethylpyridine (102.26 mg, 0.452 mmol), 1,4-dioxane (3 mL), copper iodide (8.58 mg, 0.0452 mmol), trans-N,N′-dimethyl-cyclohexyl-1,2-diamine (19.25 mg, 0.135 mmol) and potassium phosphate (286.56 mg, 1.35 mmol) in a vial at 115° C. overnight under nitrogen atmosphere to afford the crude product. Purification by preparative HPLC afforded 15 mg of the product (9.09% yield).

후처리

  1. customto afford the crude product
  2. customPurification by preparative HPLC

출처 및 근거

ORD 기록
ord-dcd7f1f103704fb89cdb17972ce49c94
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946260B2

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