3-(4-Bromothiophenoxy)propionic acid → 6-Bromo-2,3-dihydro-4H-1-benzothiopyran-4-one

HRID 617694노트

반응식

HRID 617694 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8][CH2:9][CH2:10][C:11]([OH:13])=O)=[CH:4][CH:3]=1>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[S:8][CH2:9][CH2:10][C:11](=[O:13])[C:6]=2[CH:7]=1

참가 물질

3

반응물 1

HCID 167762423-(4-Bromothiophenoxy)propionic acid

생성물 1

HCID 139537366-Bromo-2,3-dihydro-4H-1-benzothiopyran-4-one수율 57.3%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

200 mL of concentrated sulfuric acid was added to 27.7 g (0.106 mol) of the title compound of Step A. The mixture was stirred at room temperature under nitrogen overnight, and was then poured over crushed ice. The mixture was filtered, and the solid was dissolved in methylene chloride. The resulting solution was dried (MgSO4), filtered, and evaporated to dryness to yield 14.77 g of the title compound of Step B as a solid melting at 50° C. (dec). 1H NMR (CDCl3): δ3.0 (m,2H), 3.2 (m,2H), 7.16-8.2 (3H).

후처리

  1. additionwas then poured
  2. customover crushed ice
  3. filtrationThe mixture was filtered
  4. dissolutionthe solid was dissolved in methylene chloride
  5. dry with materialThe resulting solution was dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-c0a96694de4947318c2af7fe7de6c114
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952266

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