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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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4-Methylpyridine → HCID 65583291, 화합물

HRID 1496625
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HRID 1496625 반응식
C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[CH3:11][C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1.[Cl:18][C:19]1[S:23][C:22]([C:24](OCC)=[O:25])=[CH:21][CH:20]=1>CCCCCC.C1COCC1>[Cl:18][C:19]1[S:23][C:22]([C:24](=[O:25])[CH2:11][C:12]2[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=2)=[CH:21][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 79634-MethylpyridineHCID 521808Ethyl 5-chlorothiophene-2-carboxylateHCID 2733832Lithium hexamethyldisilazane

생성물 1

HCID 65583291HCID 65583291, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8058Hexane용매

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온도
5 °C

실험 절차

At 0° C., 64.5 ml of a 1M solution of lithium bis(trimethylsilyl)amide in hexane are added dropwise to a solution of 3.00 g (32.3 mmol) of 4-methylpyridine and 6.77 g (35.5 mmol) of ethyl 5-chlorothiophene-2-carboxylate in 58 ml THF, and the reaction mixture is stirred at 5° C. for 3 h. The resulting precipitate was filtered off, acidified with 6M HCl, filtered again and dried. This gives 2.9 g (35%) of the desired product; 1H-NMR (DMSO-d6): δ=8.53 (d, 2H), 8.09 (d, 1H), 7.40 (d, 1H), 7.34 (d, 2H), 4.39 (s, 2H).

후처리

  1. filtrationThe resulting precipitate was filtered off
  2. filtrationfiltered again
  3. customdried

출처 및 근거

ORD 기록
ord-2559aebc93ea47b19234463dba5e3caa
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09198426B2

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