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Tributylamine → HCID 15136782, 화합물

HRID 893641
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HRID 893641 반응식
[CH3:1][C:2]1[CH:6]=[C:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])[NH:4][N:3]=1.CS(O[CH2:17][CH:18]1[CH2:20][CH2:19]1)(=O)=O.C(N(CCCC)CCCC)CCC>C(OCC)C>[CH:18]1([CH2:17][N:4]2[C:5]([C:7]([O:9][CH2:10][CH3:11])=[O:8])=[CH:6][C:2]([CH3:1])=[N:3]2)[CH2:20][CH2:19]1
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참가 물질

5

반응물 3

HCID 7622TributylamineHCID 135444Cyclopropylmethyl methanesulfonateHCID 178469061HCID 178469061, 화합물

생성물 1

HCID 15136782HCID 15136782, 화합물수율 54.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture comprising 3.8 g of ethyl 3-methyl-1H-pyrazole-5-carboxylate, 3.8 g of cyclopropylmethyl methanesulfonate and 4.6 g of tri-n-butylamine was allowed to react at 110 ° C. for three hours without using any solvent. Then the reaction mixture was allowed to cool and diethyl ether was added thereto. The obtained mixture was successively washed with 1 N hydrochloric acid, an aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by column chromatography (eluent: hexane:ethyl acetate=14 : 1). Thus 0.62 g of the aimed ethyl 1-cyclobutyl-3-methyl-1H-pyrazole-5-carboxylate (compound No. 1001) (yield: 12.1 %) and 2.45 g of ethyl 1-cyclopropylmethyl-3-methyl-1H-pyrazole-5-carboxylate (yield: 54.3 %) were obtained.

후처리

  1. customto react at 110 ° C. for three hours
  2. temperatureto cool
  3. washThe obtained mixture was successively washed with 1 N hydrochloric acid
  4. dry with materialan aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt and then dried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe obtained residue was purified by column chromatography (eluent: hexane:ethyl acetate=14 : 1)

출처 및 근거

ORD 기록
ord-4a45922bb6d34692abfa2103497f4beb
출처 데이터셋
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05126362

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