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1,3-Dibromopropane → HCID 21963798, 화합물

HRID 2212065
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HRID 2212065 반응식
[Li].C1(S([C:11]2([S:15]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)(=[O:17])=[O:16])[CH2:14][CH2:13][CH2:12]2)(=O)=O)C=CC=CC=1.[Br:24][CH2:25][CH2:26][CH2:27]Br>O1CCCC1>[Br:24][CH2:25][CH2:26][CH2:27][C:11]1([S:15]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)(=[O:16])=[O:17])[CH2:12][CH2:13][CH2:14]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 80011,3-DibromopropaneHCID 3028194LithiumHCID 118098431,1-Bis(phenylsulfonyl)cyclobutane

생성물 1

HCID 21963798HCID 21963798, 화합물수율 65%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium napthtalenide in tetrahydrofuran (4.3M, 60 ml) was added to a stirred solution of 1,1-bis(phenylsulfonyl)cyclobutane (4.15 g, 12.35 mmol) at −78° C. over 20 min. The mixture was stirred for 15 min. and 1,3-dibromopropane (10 ml) was added in one portion. The cold bath was removed and the mixture was stirred at ambient temperature for 2 hours. The reaction mixture was treated with saturated aqueous ammonium chloride solution and extracted into ethyl acetate. The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated. The residue was purified on silica gel to give the title product (2.55 g, 65%).

후처리

  1. customThe cold bath was removed
  2. stirringthe mixture was stirred at ambient temperature for 2 hours
  3. additionThe reaction mixture was treated with saturated aqueous ammonium chloride solution
  4. extractionextracted into ethyl acetate
  5. washThe combined organic extracts were washed with brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated
  8. customThe residue was purified on silica gel

출처 및 근거

ORD 기록
ord-41ce711b69f0474ca476e181a4a36a3d
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07101892B2

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