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Ethyl Acetate → HCID 59678697, 화합물

HRID 1751870
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HRID 1751870 반응식
[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH2:12][O:13][Si:14]([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15])=[C:8](Cl)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2].C(=O)([O-])[O-].[Cs+].[Cs+].[C:28]([C:32]1[CH:39]=[CH:38][C:35]([CH2:36][SH:37])=[CH:34][CH:33]=1)([CH3:31])([CH3:30])[CH3:29].C(OCC)(=O)C>CN(C=O)C>[C:1]([N:5]1[C:10](=[O:11])[C:9]([CH2:12][O:13][Si:14]([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15])=[C:8]([S:37][CH2:36][C:35]2[CH:38]=[CH:39][C:32]([C:28]([CH3:31])([CH3:30])[CH3:29])=[CH:33][CH:34]=2)[CH:7]=[N:6]1)([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 10796Cesium carbonateHCID 27572524-tert-Butylbenzyl mercaptanHCID 59678615HCID 59678615, 화합물

생성물 1

HCID 59678697HCID 59678697, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

To a solution of 2-tert-butyl-4-tert-butyldimethylsilyloxymethyl-5-chloro 3(2H)-pyridazinone (1.5 g, 4.54 mmol) in DMF (10 ml) is added anhydrous cesium carbonate (2.9 g, 9.09 mmol) and 4-tert-butybenzyl mercaptan (1.02 g, 4.54 mmol). The mixture is stirred for 2 hours at 70° C. and then cooled to room temperature and ethyl acetate is added to it. The solution is then washed with water, dried and concentrated and the residue subjected to purification by flash chromatography (silica gel; ethyl acetate/hexanes) to give the above compound.

후처리

  1. temperaturecooled to room temperature
  2. washThe solution is then washed with water
  3. customdried
  4. concentrationconcentrated
  5. customthe residue subjected to purification by flash chromatography (silica gel; ethyl acetate/hexanes)
  6. customto give the above compound

출처 및 근거

ORD 기록
ord-1626f8f7ff5c4f1590d3af07ab0d0a92
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09161997B2

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