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Butyl bromide → 2-Butyl-1,3-dithiane

HRID 65811
ノート
印刷プレビュー

反応式

HRID 65811 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8002Butyl bromideHCID 8028Tetrahydrofuran2 回HCID 104511,3-DithianeHCID 178418339Butyllithium

生成物 1

HCID 6379752-Butyl-1,3-dithiane

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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:

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-21400c26edc047e9a8a0994dfa4c8ee8
出典データセット
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04128720

反応ノート

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