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Chlorine → HCID 178478025, 화합물

HRID 1376319
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HRID 1376319 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:12]=[CH:11][NH:10][N:9]=1.[Cl:13]Cl>C(O)(=O)C.C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([Cl:13])=[CH:11][NH:10][N:9]=1
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참가 물질

5

반응물 2

HCID 24526ChlorineHCID 178478013HCID 178478013, 화합물

생성물 1

HCID 178478025HCID 178478025, 화합물수율 44.5%

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 6344Dichloromethane용매

실험 절차

6.8 g (0.038 mol) of 3-(2'-chlorophenyl)-1H-pyrazole, prepared as in Example 9, are dissolved, at temperature and with stirring, in 30 ml of acetic acid. 2.9 g (0.0409 mol) of chlorine are then introduced into the reaction mixture. Stirring is maintained for 1 hour at room temperature and then the acetic acid is driven off under reduced pressure. The residue is taken up in methylene chloride and this organic solution is washed with in aqueous bicarbonate solution, then with water and then dried over Na2SO4 before being concentrated to dryness. The residue is chromatographed on a silica column (eluent: heptane/ethyl acetate 60/40). 3.6 g of 3-(2'-chlorophenyl)-4-chloro-1H-pyrazole (compound 96) are obtained, which is of honey-like consistency (yield 44%).

후처리

  1. dissolutionare dissolved, at temperature
  2. washthis organic solution is washed with in aqueous bicarbonate solution
  3. dry with materialwith water and then dried over Na2SO4
  4. concentrationbefore being concentrated to dryness
  5. customThe residue is chromatographed on a silica column (eluent: heptane/ethyl acetate 60/40)

출처 및 근거

ORD 기록
ord-44e8366371f34efb9606df81416b8b9a
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05663119

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