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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 54452402, 화합물

HRID 1440982
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HRID 1440982 반응식
[CH3:1][C:2]1[C:7]([C:8](OC)=[O:9])=[C:6]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[C:5]([C:19](OC)=[O:20])=[C:4]([CH3:23])[N:3]=1.O>C1(C)C=CC=CC=1.O1CCCC1>[OH:9][CH2:8][C:7]1[C:2]([CH3:1])=[N:3][C:4]([CH3:23])=[C:5]([CH2:19][OH:20])[C:6]=1[C:12]1[CH:13]=[CH:14][C:15]([F:18])=[CH:16][CH:17]=1
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참가 물질

5

반응물 2

HCID 962WaterHCID 735523Dimethyl 4-(4-fluorophenyl)-2,6-dimethylpyridine-3,5-dicarboxylate

생성물 1

HCID 54452402HCID 54452402, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8028Tetrahydrofuran용매

실험 절차

25 ml (87.5 mmol) of a 3.5 molar solution of sodium bis-(2-methoxyethoxy)-dihydroaluminate in toluene are added under nitrogen to a solution of 7.9 g (25 mmol) of the compound from Example 19 in 100 ml of dry tetrahydrofuran at 0° C. The mixture is stirred at room temperature for 6 h, cooled again to 0° C. and 200 ml of water are slowly added dropwise. The mixture is extracted three times using 150 ml of ethyl acetate each time, the combined organic phases are washed once with saturated sodium chloride solution, dried over magnesium sulphate and concentrated in vacuo. The residue is stirred with ether, filtered off with suction and dried in a desiccator.

후처리

  1. temperaturecooled again to 0° C.
  2. extractionThe mixture is extracted three times
  3. washthe combined organic phases are washed once with saturated sodium chloride solution
  4. dry with materialdried over magnesium sulphate
  5. concentrationconcentrated in vacuo
  6. stirringThe residue is stirred with ether
  7. filtrationfiltered off with suction
  8. customdried in a desiccator

출처 및 근거

ORD 기록
ord-b473996cb6144d02b13ad8d5470bd4d0
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05502057

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