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Water → HCID 19976910, 화합물

HRID 1440345
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HRID 1440345 반응식
[C:1]1([C:7]2[CH:11]=[CH:10][S:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH2:12].C(Cl)(Cl)Cl>O1CCCC1>[C:1]1([C:7]2[CH:11]=[C:10]([CH:6]([OH:12])[CH2:1][CH2:2][CH3:3])[S:9][N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

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HCID 962WaterHCID 6212ChloroformHCID 5950443-Phenylisothiazole

생성물 1

HCID 19976910HCID 19976910, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Dissolved in 60 ml of anhydrous tetrahydrofuran were 3.1 g (19.1 mmol) of 3-phenylisothiazole, followed by the addition 18.2 ml of an n-butyl lithium-hexane solution (1.57 mol/l) under a nitrogen gas stream at -78° C. over a dry ice-acetone bath. After the resulting mixture was stirred for 1 hour, 1.51 g (21 mmol) of butylaldehyde were added dropwise. The solution was stirred for 1 hour at the same temperature, whereby the reaction was completed. Water and chloroform were added. The reaction product was extracted into an organic layer. The organic layer was concentrated and the concentrate was purified by silica gel chromatography (eluent: 20:1 n-hexane/ethyl acetate), so that 3-phenyl-5-(1-hydroxybutyl)isothiazole was obtained as yellow oil.

후처리

  1. additionfollowed by the addition 18.2 ml of an n-butyl lithium-hexane solution (1.57 mol/l) under a nitrogen gas stream at -78° C. over a dry ice-acetone bath
  2. stirringThe solution was stirred for 1 hour at the same temperature, whereby the reaction
  3. extractionThe reaction product was extracted into an organic layer
  4. concentrationThe organic layer was concentrated
  5. customthe concentrate was purified by silica gel chromatography (eluent: 20:1 n-hexane/ethyl acetate), so that 3-phenyl-5-(1-hydroxybutyl)isothiazole
  6. customwas obtained as yellow oil

출처 및 근거

ORD 기록
ord-07d828cba11343a18701207cbf0d4754
출처 데이터셋
uspto-grants-1996_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05498619

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