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Acetic Acid → 3-[4-[3-(Benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-propionic acid

HRID 1934740
ノート
印刷プレビュー

反応式

HRID 1934740 の反応式
[CH2:1]([O:8][C:9](=[O:32])[CH2:10][CH2:11][N:12]1[C:16]2([CH2:21][CH2:20][C:19](=[CH:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:18][CH2:17]2)[S:15][CH:14]([CH2:27]C(O)=O)[C:13]1=[O:31])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)(Cl)=O.O.[C:38]([OH:41])(=[O:40])[CH3:39]>C(Cl)Cl.C(OCC)(=O)C>[CH2:1]([O:8][C:9](=[O:32])[CH2:10][CH2:11][N:12]1[C:16]2([CH2:17][CH2:18][C:19](=[CH:22][CH2:23][CH:24]([CH3:26])[CH3:25])[CH2:20][CH2:21]2)[S:15][CH:14]([CH2:27][CH2:39][C:38]([OH:41])=[O:40])[C:13]1=[O:31])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 24386Thionyl ChlorideHCID 224671502-[4-[3-(Benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetic acid

生成物 1

HCID 224671773-[4-[3-(Benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-propionic acid

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

In 10 ml of methylene chloride was dissolved 0.96 g of 2-[4-[3-(benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-acetic acid. After adding 0.18 ml of thionyl chloride at ambient temperature, the resulting mixture was stirred for one hour under reflux. The reaction mixture was concentrated under reduced pressure, and the concentrate was dissolved in 10 ml of dioxane. The resulting solution was dropwise added at 0-5° C. to an ethyl ether solution containing diazomethane prepared from 5.00 g of N-methylnitrosourea, 3.00 g of potassium hydroxide, 4.00 ml of water and 15 ml of ethyl ether, and the resulting mixture was stirred at ambient temperature for 30 minutes. The reaction mixture was poured into a mixture of water, acetic acid and ethyl acetate, and the organic layer was separated. The organic layer thus obtained was washed successively with water, saturated aqueous solution of sodium hydrogen carbonate and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was dissolved in a mixture of 10 ml dioxane and 10 ml water, and the resulting solution was added to a mixture of 0.16 g of silver benzoate and 3.00 ml of triethylamine at ambient temperature and stirred for 2 hours. The reaction mixture was poured into a mixture of water and ethyl acetate, pH was adjusted to 2.0 with 2 mol/L hydrochloric acid, and the organic layer was separated. The organic layer thus obtained was washed successively with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by column chromatography [eluent: chloroform:ethanol=80:1] gave 0.36 g of 3-[4-[3-(benzyloxy)-3-oxopropyl]-8-(3-methylbutylidene)-3-oxo-1-thia-4-azaspiro[4.5]decan-2-yl]-propionic acid as a light yellow oily product.

後処理

  1. temperatureunder reflux
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe concentrate was dissolved in 10 ml of dioxane
  4. additionThe resulting solution was dropwise added at 0-5° C. to an ethyl ether solution
  5. additioncontaining diazomethane
  6. customprepared from 5.00 g of N-methylnitrosourea, 3.00 g of potassium hydroxide, 4.00 ml of water and 15 ml of ethyl ether
  7. stirringthe resulting mixture was stirred at ambient temperature for 30 minutes
  8. customthe organic layer was separated
  9. customThe organic layer thus obtained
  10. washwas washed successively with water, saturated aqueous solution of sodium hydrogen carbonate and saturated aqueous solution of sodium chloride
  11. dry with materialdried over anhydrous magnesium sulfate
  12. distillationthe solvent was distilled off under reduced pressure
  13. dissolutionThe residue was dissolved in a mixture of 10 ml dioxane and 10 ml water
  14. additionthe resulting solution was added to a mixture of 0.16 g of silver benzoate and 3.00 ml of triethylamine at ambient temperature
  15. stirringstirred for 2 hours
  16. additionThe reaction mixture was poured into a mixture of water and ethyl acetate, pH
  17. customthe organic layer was separated
  18. customThe organic layer thus obtained
  19. washwas washed successively with water and saturated aqueous solution of sodium chloride
  20. dry with materialdried over anhydrous magnesium sulfate
  21. distillationthe solvent was distilled off under reduced pressure
  22. customPurification of the residue by column chromatography [eluent: chloroform:ethanol=80:1]

出典と根拠

ORDレコード
ord-58a9ba8809bb4afb960dcb78fc7c7f97
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06384065B1

反応ノート

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