Potassium Carbonate → HCID 14695585、化合物

HRID 619893ノート

反応式

HRID 619893 の反応式
[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]C(OC)=O)=[CH:4][C:3]=1[N:14]1[C:18](=[O:19])[C:17](=[C:20]([CH3:22])[CH3:21])[O:16][C:15]1=[O:23].C(=O)([O-])[O-].[K+].[K+]>CO>[F:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:14]1[C:18](=[O:19])[C:17](=[C:20]([CH3:21])[CH3:22])[O:16][C:15]1=[O:23]

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 14695618HCID 14695618、化合物

生成物 1

HCID 14695585HCID 14695585、化合物収率 56%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a dried methanol solution (100 ml) of 3-(2'-fluoro-4'-chloro-5'-methoxycarbonyloxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (3.44 g, 10 mmol), which was synthesized by a method shown in Reference Example 12 described below, was added potassium carbonate (1.38 g, 10 mmol) and the mixture was heated at reflux for 2 hours. After the reaction was completed, the resulting mixture was quenched with an aqueous solution of ammonium chloride and extracted with ether. The ethereal extracts were dried and evaporated as small a volume as possible. The resulting residue was purified by silica gel column chromatography to give pure 3-(2'-fluoro-4'-chloro-5'-hydroxyphenyl)-5-isopropylidene-1,3-oxazolidine-2,4-dione (1.60 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 hours
  3. customthe resulting mixture was quenched with an aqueous solution of ammonium chloride
  4. extractionextracted with ether
  5. customThe ethereal extracts were dried
  6. customevaporated as small a volume as possible
  7. customThe resulting residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-60e8a624e39c4e308aea2683648e23c4
出典データセット
uspto-grants-1989_04
特許番号
US04818272

反応ノート

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