Hydrochloric Acid → HCID 66761804, 화합물

HRID 573782

반응식

HRID 573782 반응식
[O:1]1[C:3]2([CH2:8][CH2:7][O:6][CH2:5][CH2:4]2)[CH2:2]1.[CH3:9][CH:10]([CH3:18])[C:11](=[O:17])[CH2:12][C:13](OC)=[O:14].[O-]CC.[Na+].Cl>C(O)C>[C:11]([CH:12]1[CH2:2][C:3]2([CH2:4][CH2:5][O:6][CH2:7][CH2:8]2)[O:1][C:13]1=[O:14])(=[O:17])[CH:10]([CH3:18])[CH3:9]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 1604391,6-Dioxaspiro[2.5]octaneHCID 2723922Sodium ethoxideHCID 2759969Methyl 4-methyl-3-oxopentanoate

생성물 1

HCID 66761804HCID 66761804, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

6.6 g 1,6-Dioxaspiro[2.5]octane and 8.2 ml methyl 4-methyl-3-oxopentanoate are dissolved in 30 ml ethanol, cooled to 0° C. and treated in portions with 3.9 g sodium ethoxide. After completion of the addition the mixture is warmed to room temperature and stirred for 18 hours. Then the mixture is poured in 200 ml ice water, acidified to pH 3 by addition of 1 M hydrochloric acid and extracted for three times with ethylacetate. The combined organic phases are dried with sodium sulphate and the solvents are evaporated in vacuo. The residue is chromatographed on silica gel (petrole ether/ethylacetate 100:0 to 50:50).

후처리

  1. additionAfter completion of the addition the mixture
  2. temperatureis warmed to room temperature
  3. extractionextracted for three times with ethylacetate
  4. dry with materialThe combined organic phases are dried with sodium sulphate
  5. customthe solvents are evaporated in vacuo
  6. customThe residue is chromatographed on silica gel (petrole ether/ethylacetate 100:0 to 50:50)

출처 및 근거

ORD 기록
ord-34528e89b8a24c86a44971d0834fbb33
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029544B2

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