Sodium Iodide → HCID 20636318、化合物

HRID 49329

反応式

HRID 49329 の反応式
CS([O:5][CH2:6][C:7]1[S:8][C:9]([C:12]2([CH2:17][CH3:18])[O:16][CH2:15][CH2:14][O:13]2)=[CH:10][CH:11]=1)(=O)=O.O[C:20]1[CH:21]=[C:22]([C:30]([O:32][CH3:33])=[O:31])[C:23](=[CH:28][CH:29]=1)[C:24]([O:26][CH3:27])=[O:25].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CC(=O)CC>[CH2:17]([C:12]1([C:9]2[S:8][C:7]([CH2:6][O:5][C:29]3[CH:28]=[C:23]([C:24]([O:26][CH3:27])=[O:25])[C:22](=[CH:21][CH:20]=3)[C:30]([O:32][CH3:33])=[O:31])=[CH:11][CH:10]=2)[O:16][CH2:15][CH2:14][O:13]1)[CH3:18]

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 89726Dimethyl 4-hydroxyphthalateHCID 206363015-(2-Ethyl-[1,3]dioxolan-2-yl)-2-thienylmethyl methanesulphonate

生成物 1

HCID 20636318HCID 20636318、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

9.25 g (43.2 mmol) of 5-(2-ethyl-[1,3]dioxolan-2-yl)-2-thienylmethyl methanesulphonate are dissolved in 100 mL of 2-butanone, and 9.07 g (43.2 mmol) of dimethyl 4-hydroxyphthalate (prepared in Example 1(b)), 6 g of potassium carbonate (43.2 mmol) and 20 mg of sodium iodide are added. The mixture is refluxed for 12 hours, cooled and filtered. The filtrate is concentrated under reduced pressure and then purified by chromatography on a column of silica. A yellow oil is obtained (m=12.70 g; Y=73%).

後処理

  1. temperatureThe mixture is refluxed for 12 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated under reduced pressure
  5. custompurified by chromatography on a column of silica
  6. customA yellow oil is obtained (m=12.70 g; Y=73%)

出典と根拠

ORDレコード
ord-3398eeb0de564ba9ab1b8cc49873e73a
出典データセット
uspto-grants-2004_03
特許番号
US06706725B1

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