Hydrochloric Acid → Texacromil

HRID 893988노트

반응식

HRID 893988 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 3086067Texacromil수율 89.8%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-df7d36e322714315860f889fb0aac1f0
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04282247

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