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1,3-Dibromopropane → HCID 21963798、化合物

HRID 2212065
ノート
印刷プレビュー

反応式

HRID 2212065 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 21963798HCID 21963798、化合物収率 65%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-41ce711b69f0474ca476e181a4a36a3d
出典データセット
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07101892B2

反応ノート

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