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Chloroform → HCID 178463143, 화합물

HRID 254208
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HRID 254208 반응식
B(Br)(Br)Br.[Cl:5][CH2:6][C:7]1([CH3:27])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([C:23]([F:26])([F:25])[F:24])=[N:16][N:17]([CH2:21][CH3:22])[C:18]=2[O:19]C)[CH2:8]1.C(Cl)(Cl)Cl>ClCCl>[Cl:5][CH2:6][C:7]1([CH3:27])[O:11][N:10]=[C:9]([S:12][CH2:13][C:14]2[C:15]([C:23]([F:26])([F:25])[F:24])=[N:16][N:17]([CH2:21][CH3:22])[C:18]=2[OH:19])[CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 25134Boron tribromideHCID 22934885HCID 22934885, 화합물

생성물 1

HCID 178463143HCID 178463143, 화합물수율 66.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

10 ml of boron tribromide (2 M/liter of dichloromethane solution, 20.2 mmoles) was added, at −60° C., into a solution of 2.5 g (6.7 mmoles) of 5-chloromethyl-3-(1-ethyl-5-methoxy-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5-meth-yl-2-isoxazoline dissolved in 30 ml of dichloromethane. The mixture was stirred at room temperature overnight to give rise to a reaction. After the completion of the reaction, the reaction mixture was poured into ice water and extraction with chloroform was conducted. The resulting organic layer was washed with water and an aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate. The resulting solution was subjected to reduced pressure distillation to remove the solvent contained therein. The residue was purified by silica gel column chromatography to obtain 1.6 g (yield: 66.7%) of 5-chloromethyl-3-(1-ethyl-5-hydroxy-3-trifluoromethyl-1H-pyrazol-4-ylmethylthio)-5-methyl-2-isoxazoline.

후처리

  1. customto give rise
  2. customto a reaction
  3. customAfter the completion of the reaction
  4. washThe resulting organic layer was washed with water
  5. dry with materialan aqueous sodium chloride solution in this order and then dried over anhydrous magnesium sulfate
  6. distillationThe resulting solution was subjected to reduced pressure distillation
  7. customto remove the solvent
  8. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-2572aa24a6624a3c8c2e01d446a2ae4f
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07875606B2

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