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

HRID 617694ノート

反応式

HRID 617694 の反応式
[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

参加物

3

反応物 1

HCID 167762423-(4-Bromothiophenoxy)propionic acid

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c0a96694de4947318c2af7fe7de6c114
出典データセット
uspto-grants-1999_09
特許番号
US05952266

反応ノート

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