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Potassium Carbonate → HCID 86692570, 화합물

HRID 1748632
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HRID 1748632 반응식
[CH3:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([CH3:13])=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1[C:14]([NH2:16])=[O:15].Br[C:18]1[CH:19]=[CH:20][C:21]([C:24]2([C:34]#[N:35])[CH2:33][CH2:32][C:27]3([O:31][CH2:30][CH2:29][O:28]3)[CH2:26][CH2:25]2)=[N:22][CH:23]=1.CN(CC)C.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.[Cu]I.O>[C:34]([C:24]1([C:21]2[N:22]=[CH:23][C:18]([NH:16][C:14]([C:3]3[CH:4]=[N:5][N:6]([C:7]4[CH:8]=[CH:9][C:10]([CH3:13])=[CH:11][CH:12]=4)[C:2]=3[CH3:1])=[O:15])=[CH:19][CH:20]=2)[CH2:25][CH2:26][C:27]2([O:28][CH2:29][CH2:30][O:31]2)[CH2:32][CH2:33]1)#[N:35]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11430Potassium CarbonateHCID 11723DimethylethylamineHCID 8080138HCID 8080138, 화합물HCID 86692457HCID 86692457, 화합물

생성물 1

HCID 86692570HCID 86692570, 화합물수율 2.6%

시약·촉매·용매 3

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

5-Methyl-1-(4-methylphenyl)-1H-pyrazole-4-carboxamide (786 mg) and 8-(5-bromopyridin-2-yl)-1,4-dioxaspiro[4.5]decane-8-carbonitrile (1.12 g) described in Reference Example 82, copper (I) iodide (35 mg), N,N-dimethylethylamine (33 mg) and potassium carbonate in 1,4-dioxane (5 ml) was stirred at 100° C. for six hours. After the reaction, water was added and extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and concentrated. The residue was purified with a silica gel column chromatography to give the titled compound (42 mg).

후처리

  1. additionwas added
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified with a silica gel column chromatography

출처 및 근거

ORD 기록
ord-7c0cd5129d224ed8b6c92092a080f973
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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