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Sodium Hydroxide → HCID 13851426, 화합물

HRID 979169
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HRID 979169 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[S:10][CH2:11][CH2:12][C:13]([OH:15])=O.[OH-].[Na+]>C(Cl)(Cl)Cl>[CH3:9][O:8][C:6]1[CH:7]=[C:2]([CH3:1])[C:3]2[S:10][CH2:11][CH2:12][C:13](=[O:15])[C:4]=2[CH:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 13851425HCID 13851425, 화합물

생성물 1

HCID 13851426HCID 13851426, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A solution of 21.1 g 3-[(2-methyl-4-methoxyphenyl)thio]propanoic acid and 160 g polyphosphoric ester in 150 ml CHCl3 is refluxed for 45 min. To the cooled reaction mixture is added 200 ml 0.5 N NaOH. The organic phase is separated and the aqueous phase is extracted with 100 ml CHCl3. The combined organic extracts are dried over Na2SO4, filtered, concentrated under reduced pressure and flash chromatrographed with ethyl acetate/hexane (8:92) to yield 6-methoxy-8-methyl-2H-[1]benzothiopyran-4-one.

후처리

  1. customTo the cooled reaction mixture
  2. customThe organic phase is separated
  3. extractionthe aqueous phase is extracted with 100 ml CHCl3
  4. dry with materialThe combined organic extracts are dried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure and flash

출처 및 근거

ORD 기록
ord-61e2149a19f14ec29612012cdcb98da1
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04666916

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