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Pyridine → HCID 11097066, 화합물

HRID 461925
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HRID 461925 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 702345-Hexyn-1-ol

생성물 1

HCID 11097066HCID 11097066, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7692b7b9ec1541ea8b7726788f8838d0
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04064257

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