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Dichloromethane → HCID 68830318, 화합물

HRID 1392868
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HRID 1392868 반응식
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH2:12][O:13][Si](C(C)(C)C)(C)C)=[C:8]([S:21][CH2:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:25][CH:24]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].[F-].C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>O>[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH2:12][OH:13])=[C:8]([S:21][CH2:22][C:23]2[CH:24]=[CH:25][C:26]([C:29]([CH3:32])([CH3:31])[CH3:30])=[CH:27][CH:28]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6344DichloromethaneHCID 2724141Tetrabutylammonium FluorideHCID 59678697HCID 59678697, 화합물

생성물 1

HCID 68830318HCID 68830318, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 15 ml round bottom flask charged with 2-tert-butyl-4-tert-butyldimethylsilyloxymethyl-5-(4-tert-butylbenzyl)thio-3(2H)-pyridazinone (2 g, 4.2 mmol) is added tetrabutylammonium fluoride solution (1M in THF, 21 ml, 21 mmol). The mixture is first stirred at room temperature for 5 hours and to it is added dichloromethane followed by water. The layers are separated and the organic layer is washed with water and dried. The organic layer is then concentrated and subjected to purification using silica gel flash chromatography (ethyl acetate/hexanes) to obtain the above compound.

후처리

  1. customThe layers are separated
  2. washthe organic layer is washed with water
  3. customdried
  4. concentrationThe organic layer is then concentrated
  5. customsubjected to purification
  6. customto obtain the above compound

출처 및 근거

ORD 기록
ord-25e55a4221594929bf1ebf5c921dc12d
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07344702B2

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