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Pyridine → HCID 11097066、化合物

HRID 461925
ノート
印刷プレビュー

反応式

HRID 461925 の反応式
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.N1C=CC=CC=1.[CH2:18]([OH:24])[CH2:19][CH2:20][CH2:21][C:22]#[CH:23]>O>[S:7]([O:24][CH2:18][CH2:19][CH2:20][CH2:21][C:22]#[CH:23])([C:4]1[CH:5]=[CH:6][C:1]([CH3:11])=[CH:2][CH:3]=1)(=[O:9])=[O:8]
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 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 702345-Hexyn-1-ol

生成物 1

HCID 11097066HCID 11097066、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In this preparation 1.0 mole of p-toluenesulfonyl chloride is dissolved in 700 ml. of pyridine at 0° C, under nitrogen, and then 0.5 mole of hex-5-yn-1-ol is added dropwise. The mixture is stirred for 2 hours and then 10 ml. of water is added slowly, keeping the temperature below 10° C. The pyridine is then removed by evaporation under vacuum and the residue poured into 1 liter of ethyl acetate, then washed twice with excess 2N aqueous hydrochloric acid, and then with water. The organic layer is separated and dried over anhydrous magnesium sulfate, filtered, and the filtrate then evaporated to dryness, under vacuum, affording hex-5-yn-1-ol tosylate.

後処理

  1. dissolutionis dissolved in 700 ml
  2. customthe temperature below 10° C
  3. customThe pyridine is then removed by evaporation under vacuum
  4. additionthe residue poured into 1 liter of ethyl acetate
  5. washwashed twice with excess 2N aqueous hydrochloric acid
  6. customThe organic layer is separated
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customthe filtrate then evaporated to dryness, under vacuum

出典と根拠

ORDレコード
ord-7692b7b9ec1541ea8b7726788f8838d0
出典データセット
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04064257

反応ノート

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