Hydrochloric Acid → Texacromil

HRID 893988ノート

反応式

HRID 893988 の反応式
[OH:1][CH:2]([CH2:21][S:22][CH3:23])[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[C:7](=[O:20])[CH:8]=[C:9]([C:15]([O:17]CC)=[O:16])[O:10]2.[OH-].[Na+].Cl>CC(C)=O>[OH:1][CH:2]([CH2:21][S:22][CH3:23])[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[C:7](=[O:20])[CH:8]=[C:9]([C:15]([OH:17])=[O:16])[O:10]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12888660Ethyl 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylate

生成物 1

HCID 3086067Texacromil収率 89.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
50 °C

実験手順

To a solution of 3.4 g of ethyl 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylate in 20 ml of acetone there is added 11 ml of N sodium hydroxide and the mixture is heated at 50° C. for 10 minutes. After evaporating the solvent under reduced pressure, 30 ml of water are added, the resulting mixture is extracted with diethyl ether, filtered on charcoal and the limpid solution thus obtained is acidified with hydrochloric acid. The product which precipitates is filtered, washed with water and dried. Thus, 2.8 g of 5-(2-hydroxy-3-methylthiopropoxy)chromone-2-carboxylic acid is obtained as dihydrate (CM 57202); m.p. 76°-79° C.

後処理

  1. customAfter evaporating the solvent under reduced pressure, 30 ml of water
  2. additionare added
  3. extractionthe resulting mixture is extracted with diethyl ether
  4. filtrationfiltered on charcoal
  5. customthe limpid solution thus obtained
  6. customThe product which precipitates
  7. filtrationis filtered
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-df7d36e322714315860f889fb0aac1f0
出典データセット
uspto-grants-1981_08
特許番号
US04282247

反応ノート

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