Potassium Carbonate → (1,4-Dibenzylpiperazin-2-yl)methanol

HRID 248453

反応式

HRID 248453 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH:15]2[C:27](OCC)=[O:28])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-].[K+].C(=O)([O-])[O-].[K+].[K+]>CCOCC>[C:7]1([CH2:13][N:14]2[CH2:19][CH2:18][N:17]([CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:16][CH:15]2[CH2:27][OH:28])[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 14797Potassium HydroxideHCID 2736402Ethyl 1,4-dibenzylpiperazine-2-carboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 10827800(1,4-Dibenzylpiperazin-2-yl)methanol収率 103.2%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A 3.06 g portion of lithium aluminum hydride in 130 ml of dry ether, with argon bubbling through the solution, was stirred at room temperature. A solution of 24.5 g of 1,4-bis(phenylmethyl)-2-piperazinecarboxylic acid, ethyl ester in 125 ml of dry ether was added, the mixture was heated at reflux for 5 hours and then cooled. A 40 ml portion of 40% aqueous potassium hydroxide followed by 80 ml of saturated aqueous potassium carbonate were added dropwise, under argon. The mixture was allowed to stand overnight, after stirring for one hour. The ether layer was removed and saved, then the remainder filtered. The filtrate was extracted several times with ether. The ether solutions were combined, dried, filtered and evaporated, giving 22.15 g of 1,4-bis(phenylmethyl)-2-piperazinemethanol as a colorless oil.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 5 hours
  3. temperaturecooled
  4. additionwere added dropwise, under argon
  5. customThe ether layer was removed
  6. filtrationthe remainder filtered
  7. extractionThe filtrate was extracted several times with ether
  8. customdried
  9. filtrationfiltered
  10. customevaporated

出典と根拠

ORDレコード
ord-a652b59fbd174400b73fe4888044c90b
出典データセット
uspto-grants-1993_05
特許番号
US05210193

関連ノート

読み込み中…