Acetic Acid → HCID 18355461、化合物

HRID 429335ノート

反応式

HRID 429335 の反応式
[CH2:1]([O:3][C:4]([CH2:6][C:7]([C:9]1[O:10][C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[CH:13]=1)=O)=[O:5])[CH3:2].[BH4-].[Na+].C(O)(=O)C>C(O)C.O.[Pd]>[O:10]1[C:11]2[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=2[CH:13]=[C:9]1[CH2:7][CH2:6][C:4]([O:3][CH2:1][CH3:2])=[O:5]

参加物

7

反応物 3

HCID 176Acetic AcidHCID 4311764Sodium borohydride2 回HCID 12777066Ethyl 3-(1-benzofuran-2-yl)-3-oxopropanoate

生成物 1

HCID 18355461HCID 18355461、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

232 g of compound 3 are dissolved in 500 ml of ethanol. Cool in ice-bath and add 100 g of sodium borohydride in 500 ml of water. Stir for 2 hours. Add acetic acid until the sodium borohydride has been neutralized. Cool the solution in ice-bath under an atmosphere of nitrogen and add 10 g of 10% Pd/C catalyst. Stir under a hydrogen atmosphere at 15PSI until the reaction is complete, as judged by TLC. Filter through celite and evaporate organic solvents. Extract with ethyl acetate. Dry over sodium sulfate. Filter. Evaporate solvent.

後処理

  1. temperatureCool in ice-bath
  2. temperatureCool the solution in ice-bath under an atmosphere of nitrogen
  3. stirringStir under a hydrogen atmosphere at 15PSI until the reaction
  4. filtrationFilter through celite
  5. customevaporate organic solvents
  6. extractionExtract with ethyl acetate
  7. dry with materialDry over sodium sulfate
  8. filtrationFilter

出典と根拠

ORDレコード
ord-5ef3d64006d046358df24148c5752c4e
出典データセット
uspto-grants-2001_11
特許番号
US06316487B1

反応ノート

読み込み中…