Hydrochloric Acid → HCID 22467174, 화합물

HRID 1934754노트

반응식

HRID 1934754 반응식
C([O:5][C:6](=[O:31])[CH2:7][N:8]1[C:12]2([CH2:17][CH2:16][C:15](=[CH:18][CH2:19][CH:20]([CH3:22])[CH3:21])[CH2:14][CH2:13]2)[S:11][CH:10]([CH2:23][C:24]([O:26][CH:27]([CH3:29])[CH3:28])=[O:25])[C:9]1=[O:30])(C)(C)C.Cl>C(OCC)C.O1CCOCC1>[CH:27]([O:26][C:24](=[O:25])[CH2:23][CH:10]1[C:9](=[O:30])[N:8]([CH2:7][C:6]([OH:31])=[O:5])[C:12]2([CH2:13][CH2:14][C:15](=[CH:18][CH2:19][CH:20]([CH3:22])[CH3:21])[CH2:16][CH2:17]2)[S:11]1)([CH3:29])[CH3:28]

참가 물질

5

반응물 2

HCID 313Hydrochloric Acid3회HCID 22467176Isopropyl 2-[4-[2-(tert-butoxy)-2-oxoethyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetate

생성물 1

HCID 22467174HCID 22467174, 화합물수율 27.7%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매3회

실험 절차

In 3 ml of diethyl ether was dissolved 0.33 g of isopropyl 2-[4-[2-(tert-butoxy)-2-oxoethyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetate. Then, 1 ml of a 5.39 mol/L solution of dry hydrogen chloride in dioxane was added and the resulting mixture was stirred at the same temperature as above for 2 hours. Further, 1 ml of 5.39 mol/L solution of dry hydrogen chloride in dioxane was added and the resulting mixture was stirred for one hour, after which 3 ml of 5.39 mol/L solution of dry hydrogen chloride in dioxane was added and the resulting mixture was stirred for one hour. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography [eluent: chloroform]. Then, hexane was added, and the deposited crystal was collected by filtration. Thus, 0.08 g of 2-[2-(2-isopropoxy-2-oxoethyl)-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-4-yl]-acetic acid was obtained as a colorless crystalline product.

후처리

  1. stirringthe resulting mixture was stirred for one hour
  2. stirringthe resulting mixture was stirred for one hour
  3. distillationThe solvent was distilled off under reduced pressure
  4. customthe residue was purified by column chromatography [eluent: chloroform]
  5. additionThen, hexane was added
  6. filtrationthe deposited crystal was collected by filtration

출처 및 근거

ORD 기록
ord-134a70e07dae457685ba66d679eff206
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06384065B1

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