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Potassium Carbonate → HCID 22180671, 화합물

HRID 1795860
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HRID 1795860 반응식
[C:1]1([C:7]#[C:8][C:9]2[CH:10]=[CH:11][C:12]([S:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)(=[O:17])=[O:16])=[N:13][CH:14]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])([O-])=O.[K+].[K+].[I-].[NH2:31][N+:32]1[CH:37]=[CH:36][N:35]=[CH:34][CH:33]=1>CN(C=O)C>[C:1]1([C:7]2[C:8]([C:9]3[CH:14]=[N:13][C:12]([S:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)(=[O:17])=[O:16])=[CH:11][CH:10]=3)=[C:33]3[CH:34]=[N:35][CH:36]=[CH:37][N:32]3[N:31]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium Carbonate3회HCID 221806601-Aminopyrazin-1-ium iodide3회HCID 22180661HCID 22180661, 화합물

생성물 1

HCID 22180671HCID 22180671, 화합물수율 53.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of 5-(phenylethynyl)-2-(phenylsulfonyl)pyridine (6.00 g) and K2CO3 (13.0 g) in DMF (120 mL) was added 1-aminopyrazin-1-ium iodide (12.6 g) and the mixture was stirred at room temperature for 1 h, then stirred at 60° C. for 8 h. To the reaction mixture was added K2CO3 (7.80 g) and 1-aminopyrazin-1-ium iodide (8.38 g) and stirred at room temperature for 1 h, then stirred at 60° C. for 12 h. To the reaction mixture was added further K2CO3 (7.80 g) and 1-aminopyrazin-1-ium iodide (8.38 g) and stirred at room temperature for 1 h, then stirred at 60° C. for 26 h. The mixture was poured into ice water and extracted with EtOAc, washed with water and brine, dried over sodium sulfate, evaporated in vacuo. The residue was purified by silica gel column chromatography (n-hexane-EtOAc 3:1 to CHCl3-MeOH 20:1) to give 2-phenyl-3-[6-(phenylsulfonyl)-3-pyridinyl]pyrazolo[1,5-a]pyrazine (4.14 g) as an amorphous solid.

후처리

  1. stirringstirred at 60° C. for 8 h
  2. stirringstirred at room temperature for 1 h
  3. stirringstirred at 60° C. for 12 h
  4. stirringstirred at room temperature for 1 h
  5. stirringstirred at 60° C. for 26 h
  6. extractionextracted with EtOAc
  7. washwashed with water and brine
  8. dry with materialdried over sodium sulfate
  9. customevaporated in vacuo
  10. customThe residue was purified by silica gel column chromatography (n-hexane-EtOAc 3:1 to CHCl3-MeOH 20:1)

출처 및 근거

ORD 기록
ord-f7ce26d48007487f902b130deb9d7092
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030121B2

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