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Sodium Hydroxide → 6,7-Dihydro-4-methyl-2-(4-chlorophenyl)-4H-pyrano[4,3-d]thiazole-4-acetic acid

HRID 258581
ノート
印刷プレビュー

反応式

HRID 258581 の反応式
[CH3:1][C:2]1([CH2:18][C:19]([O:21]CC)=[O:20])[C:10]2[S:9][C:8]([C:11]3[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=3)=[N:7][C:6]=2[CH2:5][CH2:4][O:3]1.[OH-].[Na+]>CO>[CH3:1][C:2]1([CH2:18][C:19]([OH:21])=[O:20])[C:10]2[S:9][C:8]([C:11]3[CH:12]=[CH:13][C:14]([Cl:17])=[CH:15][CH:16]=3)=[N:7][C:6]=2[CH2:5][CH2:4][O:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 54049665ethyl 6,7-dihydro-4-methyl-2-(4-chlorphenyl)-4H-pyrano[4,3-d]thiazole-4-acetate

生成物 1

HCID 124290066,7-Dihydro-4-methyl-2-(4-chlorophenyl)-4H-pyrano[4,3-d]thiazole-4-acetic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The latter ester is dissolved in methanol (500 ml) followed by the addition of sodium hydroxide (80 g) and the resulting mixture is heated at reflux temperature for 5 hr. The solvent is removed by distillation, water is added to the residue and the solution is extracted with ether. The aqueous basic phase is mixed with ether and the mixture is acidified with dilute hydrochloric acid. The organic phase is separated, washed with saturated sodium chloride solution, dried over sodium sulfate, and evaporated under reduced pressure. The residue is crystallized from chloroform-ether to give the title compound; mp 162°-164° C., γmaxCHCl3 2900 and 1705 cm-1.

後処理

  1. temperaturethe resulting mixture is heated
  2. temperatureat reflux temperature for 5 hr
  3. customThe solvent is removed by distillation, water
  4. additionis added to the residue
  5. extractionthe solution is extracted with ether
  6. additionThe aqueous basic phase is mixed with ether
  7. customThe organic phase is separated
  8. washwashed with saturated sodium chloride solution
  9. dry with materialdried over sodium sulfate
  10. customevaporated under reduced pressure
  11. customThe residue is crystallized from chloroform-ether

出典と根拠

ORDレコード
ord-e090f359157a480ca1492a002bdf5f00
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04033977

反応ノート

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