Sodium Hydroxide → HCID 21454861、化合物

HRID 435960ノート

反応式

HRID 435960 の反応式
[OH-].[Na+].[S:3]1[CH2:8][CH2:7][S:6][CH:5]=[C:4]1[CH2:9][C:10]([O:12]CC)=[O:11]>C(O)C>[S:3]1[CH2:8][CH2:7][S:6][CH:5]=[C:4]1[CH2:9][C:10]([OH:12])=[O:11]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 54253145HCID 54253145、化合物

生成物 1

HCID 21454861HCID 21454861、化合物収率 78.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

10N Sodium hydroxide solution (71.4 cc.) is added to a solution of ethyl (5,6-dihydro-1,4-dithiin-2-yl)acetate (121.3 g.) in ethanol (800 cc.). The reaction mixture is heated for 3 hours at about 50° C. After evaporating the solvent under reduced pressure (25 mm.Hg), the residue is dissolved in distilled water (500 cc.). The alkaline aqueous solution is washed twice with ether (total 100 cc.), treated with decolourizing charcoal (0.2 g.), filtered and then acidified with excess hydrochloric acid (d = 1.19). The oil which separates out is extracted three times with diethyl ether (total 450 cc.). The combined ether solutions are washed three times with distilled water (total 300 cc.), dried over anhydrous magnesium sulphate and evaporated. The residue (102.2 g.) is dissolved in boiling diisopropyl ether (150 cc.) and then petroleum ether (b.p. 40°-60° C.) (50 cc.) is added. After 3 hours at 2° C., the crystals which have appeared are filtered off, washed twice with ice-cold diisopropyl ether (total 60 cc.) and dried under reduced pressure (25 mm.Hg) to give (5,6-dihydro-1,4-dithiin-2-yl)acetic acid (82.2 g.) melting at 82° C.

後処理

  1. customAfter evaporating the solvent under reduced pressure (25 mm.Hg)
  2. dissolutionthe residue is dissolved in distilled water (500 cc.)
  3. washThe alkaline aqueous solution is washed twice with ether (total 100 cc.)
  4. additiontreated with decolourizing charcoal (0.2 g.)
  5. filtrationfiltered
  6. extractionThe oil which separates out is extracted three times with diethyl ether (total 450 cc.)
  7. washThe combined ether solutions are washed three times with distilled water (total 300 cc.)
  8. dry with materialdried over anhydrous magnesium sulphate
  9. customevaporated
  10. dissolutionThe residue (102.2 g.) is dissolved
  11. additionpetroleum ether (b.p. 40°-60° C.) (50 cc.) is added
  12. filtrationthe crystals which have appeared are filtered off
  13. washwashed twice with ice-cold diisopropyl ether (total 60 cc.)
  14. customdried under reduced pressure (25 mm.Hg)

出典と根拠

ORDレコード
ord-7ae566bd034b43fc9111dc96245c1a4f
出典データセット
uspto-grants-1977_02
特許番号
US04007176

反応ノート

読み込み中…