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Potassium Carbonate → HCID 17842074, 화합물

HRID 645338
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HRID 645338 반응식
[CH:1]1([C:5]([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)=O)[CH2:4][CH2:3][CH2:2]1.O.NN.C([O-])([O-])=O.[K+].[K+]>C(O)COCCO>[CH:1]1([CH2:5][C:7]2[CH:8]=[CH:9][C:10]([O:13][CH3:14])=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 24654Hydrazine hydrate (1:1)HCID 13813654Cyclobutyl(4-methoxyphenyl)methanone

생성물 1

HCID 17842074HCID 17842074, 화합물수율 95%

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

실험 절차

A mixture of compound (G) (5.00 g), hydrazine hydrate (4.12 g), K2CO3 (7.00 g) and diethylene glycol (16 ml) were heated to reflux temperature for 1 hour. The condenser was exchanged by a distillation device and the mixture was distilled at 220-230° C. The distillate was extracted with MTBE and the organic phase washed with water and brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography to yield a colorless oil (4.4 g).

후처리

  1. temperaturewere heated
  2. temperatureto reflux temperature for 1 hour
  3. distillationthe mixture was distilled at 220-230° C
  4. extractionThe distillate was extracted with MTBE
  5. washthe organic phase washed with water and brine
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-5303ce8b359346df922f13f96f7808d8
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07704942B2

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