Lithium hydroxide, monohydrate → HCID 14748625、化合物

HRID 1074181ノート

反応式

HRID 1074181 の反応式
[Cl:1][C:2]1[C:10]2[O:9][CH:8]([C:11]([O:13]CC)=[O:12])[O:7][C:6]=2[CH:5]=[C:4]([C:16]([C:18]2[N:22]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)[N:21]=[CH:20][CH:19]=2)=[O:17])[C:3]=1[Cl:29].O.[OH-].[Li+]>O1CCCC1.O>[Cl:1][C:2]1[C:10]2[O:9][CH:8]([C:11]([OH:13])=[O:12])[O:7][C:6]=2[CH:5]=[C:4]([C:16]([C:18]2[N:22]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][N:24]=3)[N:21]=[CH:20][CH:19]=2)=[O:17])[C:3]=1[Cl:29]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 14748612HCID 14748612、化合物

生成物 1

HCID 14748625HCID 14748625、化合物収率 96.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1.5 g of ethyl 4,5-dichloro-6-(1-[2-pyridyl]-5-pyrazolylcarbonyl)-1,3-benzodioxole-2-carboxylate are dissolved in a mixture of 18 ml of tetrahydrofuran and 2 ml of water. 177 mg of lithium hydroxide monohydrate are added to the solution and the mixture is stirred at room temperature for one hour. The reaction mixture is concentrated under reduced pressure to remove tetrahydrofuran. Water and 1N hydrochloric acid are added to the residue, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried and evaporated under reduced pressure to remove solvent. The residue is recrystallized from ethyl acetate-n-hexane to give 1.35 g of 4,5-dichloro-6-[1-(2-pyridyl)-5-pyrazolylcarbonyl]-1,3-benzodioxole-2-carboxylic acid. Yield: 96%

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customto remove tetrahydrofuran
  3. additionWater and 1N hydrochloric acid are added to the residue
  4. extractionthe mixture is extracted with ethyl acetate
  5. washThe extract is washed with water
  6. customdried
  7. customevaporated under reduced pressure
  8. customto remove solvent
  9. customThe residue is recrystallized from ethyl acetate-n-hexane

出典と根拠

ORDレコード
ord-7a7fe3d37e2d4a04a321cea995788439
出典データセット
uspto-grants-1990_11
特許番号
US04973600

反応ノート

読み込み中…