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Butyl bromide → 2-Butyl-1,3-dithiane

HRID 65811
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HRID 65811 반응식
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[S:6]1[CH2:11][CH2:10][CH2:9][S:8][CH2:7]1.O1CCCC1.C(Br)CCC>CCCCCC>[CH2:1]([CH:7]1[S:8][CH2:9][CH2:10][CH2:11][S:6]1)[CH2:2][CH2:3][CH3:4]
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참가 물질

6

반응물 4

HCID 8002Butyl bromideHCID 8028Tetrahydrofuran2회HCID 104511,3-DithianeHCID 178418339Butyllithium

생성물 1

HCID 6379752-Butyl-1,3-dithiane

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

30 ml. of a 1.6M solution of n-butyllithium in n-hexane were added dropwise to a solution of 4.8 g. of 1,3-dithiane in 150 ml. of tetrahydrofuran under an atmosphere of nitrogen at -20° to -25° C. After 2 hours stirring, 6 g. of n-butyl bromide in 60 ml. of tetrahydrofuran were added dropwise to the reaction mixture, which was stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture and then concentrated under reduced pressure. The residue was dissolved in diethyl ether, washed with water and an aqueous solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure to give 6.8 g. of the title compound having the following physical characteristics:

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후처리

  1. customat -20° to -25° C
  2. stirringwas stirred for 1 hour at -20° to -25° C. and for a further 30 minutes at room temperture
  3. concentrationconcentrated under reduced pressure
  4. dissolutionThe residue was dissolved in diethyl ether
  5. washwashed with water
  6. dry with materialan aqueous solution of sodium chloride, dried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customto give 6.8 g

출처 및 근거

ORD 기록
ord-21400c26edc047e9a8a0994dfa4c8ee8
출처 데이터셋
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04128720

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