1-(1-Naphthyl)piperazine → HCID 22464422, 화합물

HRID 1935383노트

반응식

HRID 1935383 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]1[CH:15]=[CH:14][C:9]2[NH:10][C:11](=[O:13])[O:12][C:8]=2[CH:7]=1.[C:16]1([N:26]2[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]2)[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[Na+].[Na+]>[I-].[Na+].C(O)(C)C>[ClH:1].[C:16]1([N:26]2[CH2:31][CH2:30][N:29]([CH2:2][CH2:3][CH2:4][CH2:5][C:6]3[CH:15]=[CH:14][C:9]4[NH:10][C:11](=[O:13])[O:12][C:8]=4[CH:7]=3)[CH2:28][CH2:27]2)[C:25]2[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 3

HCID 13421-(1-Naphthyl)piperazineHCID 10340Sodium CarbonateHCID 14581391HCID 14581391, 화합물

생성물 1

HCID 22464422HCID 22464422, 화합물수율 497.9%

시약·촉매·용매 2

HCID 5238Sodium Iodide촉매HCID 3776Isopropanol용매

실험 절차

To a 100 ml round-bottom flask equipped with condenser and nitrogen inlet were added 0.658 grams (3.10 mmol) of 6-(4-chlorobutyl)-benzoxazolone, 0.7 grams (3.10 mmol) of N-(1-naphthyl)piperazine, 0.328 grams sodium carbonate, 2 mg sodium iodide, and 50 ml isopropanol. The reaction was refluxed for 3 days, evaporated, taken up in methylene chloride, washed with water, dried over sodium sulfate, and evaporated. The residue was chromatographed on silica gel using ethyl acetate as eluent, and the product dissolved in acetone, precipitated with ethereal HCl, and the white solid filtered, washed with acetone, and dried to afford 6.76 grams (46.0%) of a white solid, m.p. 231°-233° C.

후처리

  1. customTo a 100 ml round-bottom flask equipped with condenser and nitrogen inlet
  2. temperatureThe reaction was refluxed for 3 days
  3. customevaporated
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe residue was chromatographed on silica gel
  8. dissolutionthe product dissolved in acetone
  9. customprecipitated with ethereal HCl
  10. filtrationthe white solid filtered
  11. washwashed with acetone
  12. customdried

출처 및 근거

ORD 기록
ord-2b2b36b226e44d55ad16ae52b44ae062
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06387904B2

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