Hydrochloric Acid → HCID 22467174、化合物

HRID 1934754ノート

反応式

HRID 1934754 の反応式
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]

参加物

5

反応物 2

HCID 313Hydrochloric Acid3 回HCID 22467176Isopropyl 2-[4-[2-(tert-butoxy)-2-oxoethyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetate

生成物 1

HCID 22467174HCID 22467174、化合物収率 27.7%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 312751,4-Dioxane溶媒3 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-134a70e07dae457685ba66d679eff206
出典データセット
uspto-grants-2002_05
特許番号
US06384065B1

反応ノート

読み込み中…