Hydrochloric Acid → HCID 178459013, 화합물

HRID 275666노트

반응식

HRID 275666 반응식
[CH3:1][C:2]1([CH3:22])[C:11]2[C:6](=[C:7]([CH2:15][O:16][CH2:17][CH2:18][CH3:19])[C:8]([C:12](O)=[O:13])=[CH:9][CH:10]=2)[S:5](=[O:21])(=[O:20])[CH2:4][CH2:3]1.[CH3:23][N:24]1[C:28]([OH:29])=[CH:27][CH:26]=[N:25]1.C(=O)([O-])[O-].[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+].Cl>C(#N)C.C(OCC)(=O)C.O.C(OCC)(=O)C>[CH3:1][C:2]1([CH3:22])[C:11]2[C:6](=[C:7]([CH2:15][O:16][CH2:17][CH2:18][CH3:19])[C:8]([C:12]([C:27]3[CH:26]=[N:25][N:24]([CH3:23])[C:28]=3[OH:29])=[O:13])=[CH:9][CH:10]=2)[S:5](=[O:20])(=[O:21])[CH2:4][CH2:3]1

참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 112903334,4-Dimethyl-8-propoxymethyl-1,1-dioxothiochromane-7-carboxylic acidHCID 178481816HCID 178481816, 화합물

생성물 1

HCID 178459013HCID 178459013, 화합물

시약·촉매·용매 3

HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매HCID 22728543Water ethylacetate용매

실험 절차

A solution of 0.6 g (1.84 mmol) of 4,4-dimethyl-8-propoxymethyl-1,1-dioxothiochromane-7-carboxylic acid, 0.18 g (1.84 mmol) of 1-methyl-5-hydroxypyrazole and 0.38 g (1.84 mmol) of N,N-dicyclohexylcarbodiimide in 20 ml of acetonitrile was stirred at room temperature for 12 hours. The reaction mixture was subsequently stirred into a mixture of ethyl acetate and 2% strength aqueous sodium carbonate solution, and the precipitate which formed was filtered off with suction. The organic phase of the filtrate was dried and the solvent was distilled off. The resulting residue was dissolved in 5 ml of 1,4-dioxane, 0.51 g (3.7 mmol) of potassium carbonate were added and the mixture was heated under reflux for 4 hours. After cooling, the reaction mixture was taken up in ethyl acetate/water, and the aqueous phase was adjusted to pH 3 using 2N hydrochloric acid and subsequently extracted with ethyl acetate. The extract was dried and the solvent was removed, giving a solid.

후처리

  1. customthe precipitate which formed
  2. filtrationwas filtered off with suction
  3. customThe organic phase of the filtrate was dried
  4. distillationthe solvent was distilled off
  5. dissolutionThe resulting residue was dissolved in 5 ml of 1,4-dioxane
  6. temperaturethe mixture was heated
  7. temperatureunder reflux for 4 hours
  8. temperatureAfter cooling
  9. extractionsubsequently extracted with ethyl acetate
  10. customThe extract was dried
  11. customthe solvent was removed
  12. customgiving a solid

출처 및 근거

ORD 기록
ord-ca51a17ce07a432b9c1203447caffd70
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06352959B1

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