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Hydrochloric Acid → 2-(2-Propanesulfonylamino-1,3-thiazol-4-yl)glyoxylic acid

HRID 1659386
ノート
印刷プレビュー

反応式

HRID 1659386 の反応式
[CH2:1]([S:4]([NH:7][C:8]1[S:9][CH:10]=[C:11]([C:13](=[O:19])[C:14]([O:16]CC)=[O:15])[N:12]=1)(=[O:6])=[O:5])[CH2:2][CH3:3].[OH-].[Na+].Cl>>[CH2:1]([S:4]([NH:7][C:8]1[S:9][CH:10]=[C:11]([C:13](=[O:19])[C:14]([OH:16])=[O:15])[N:12]=1)(=[O:6])=[O:5])[CH2:2][CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 20254346Ethyl 2-(2-propanesulfonylamino-1,3-thiazol-4-yl)glyoxylateHCID 178461072HCID 178461072、化合物

生成物 1

HCID 202543652-(2-Propanesulfonylamino-1,3-thiazol-4-yl)glyoxylic acid

実験手順

A mixture of ethyl 2-(2-propanesulfonylamino-1,3-thiazol-4-yl)glyoxylate, which can be represented as ethyl 2-(2-propanesulfonylimino-2,3-dihydro-1,3-thiazol-4-yl)glyoxylate, (12.0 g.) and 1 N sodium hydroxide aqueous solution (93 ml.) was stirred for 1 hour under ice-cooling. After the reaction, to the reaction mixture was added 1 N hydrochloric acid (93 ml.) and the mixture was extracted with ethyl acetate under saturation with sodium chloride. The extract was washed with a saturated aqueous solution of sodium chloride and dried. The solvent was distilled off from the extract, and the residue was washed in diethyl ether, collected by filtration and dried to give 2-(2-propanesulfonylamino-1,3-thiazol-4-yl)glyoxylic acid, which can be represented as 2-(2-propanesulfonylimino-2,3-dihydro-1,3-thiazol-4-yl)glyoxylic acid, (7.3 g.), mp. 148° to 150° C.

後処理

  1. temperaturecooling
  2. customAfter the reaction
  3. extractionthe mixture was extracted with ethyl acetate under saturation with sodium chloride
  4. washThe extract was washed with a saturated aqueous solution of sodium chloride
  5. customdried
  6. distillationThe solvent was distilled off from the extract
  7. washthe residue was washed in diethyl ether
  8. filtrationcollected by filtration
  9. customdried

出典と根拠

ORDレコード
ord-9a77e68a029e4a4c8ed44c029a0c3091
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04303655

反応ノート

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