Hydrochloric Acid → HCID 66761804、化合物

HRID 573782

反応式

HRID 573782 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 66761804HCID 66761804、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-34528e89b8a24c86a44971d0834fbb33
出典データセット
uspto-grants-2015_05
特許番号
US09029544B2

関連ノート

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