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Potassium Phosphate, Tribasic → HCID 89963353, 화합물

HRID 1843945
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HRID 1843945 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:14][C:8]3[C:9](=[O:13])[NH:10][CH2:11][CH2:12][C:7]=3[C:6]=2[CH:15]=1.I[C:17]1[CH:18]=[N:19][CH:20]=[CH:21][C:22]=1[CH3:23].[O-]P([O-])([O-])=O.[K+].[K+].[K+].CN[C@@H]1CCCC[C@H]1NC>[Cu]I.O1CCOCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:14][C:8]3[C:9](=[O:13])[N:10]([C:17]4[CH:18]=[N:19][CH:20]=[CH:21][C:22]=4[CH3:23])[CH2:11][CH2:12][C:7]=3[C:6]=2[CH:15]=1
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참가 물질

7

반응물 4

HCID 62657Potassium Phosphate, TribasicHCID 2733821trans-N,N'-dimethyl-1,2-cyclohexanediamineHCID 144235133-Iodo-4-methylpyridineHCID 89964359HCID 89964359, 화합물

생성물 1

HCID 89963353HCID 89963353, 화합물수율 37.81%

시약·촉매·용매 2

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

6-Fluoro-3,4-dihydro-2H-benzo[4,5]thieno[2,3-c]pyridin-1-one (I-45e: 85 mg, 0.384 mmol) was reacted with 3-iodo-4-methyl-pyridine (101 mg, 0.461 mmol), K3PO4 (244 mg, 1.152 mmol), trans-N,N′-dimethyl-cyclohexane-1,2-diamine (16.3 mg, 0.115 mmol), CuI (7.2 mg, 0.038 mmol) and 1,4-dioxane (10 mL). The resulting mixture was refluxed at 120° C. overnight to afford the crude product. Purification by column chromatography on silica gel (2% methanol in chloroform) afforded 45 mg of the product (37.81% yield).

후처리

  1. customto afford the crude product
  2. customPurification by column chromatography on silica gel (2% methanol in chloroform)

출처 및 근거

ORD 기록
ord-63aaedf98b584b989da0aa6b5fc26901
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946260B2

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