Chlorotrimethylsilane → 1-Ethoxycarbonyl-4-trimethylsilylpiperazine

HRID 1462444ノート

反応式

HRID 1462444 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5])[CH3:2].C([Li])CCC.Cl[Si:18]([CH3:21])([CH3:20])[CH3:19]>O1CCCC1.CCCCCC>[CH2:1]([O:3][C:4]([N:6]1[CH2:7][CH2:8][N:9]([Si:18]([CH3:21])([CH3:20])[CH3:19])[CH2:10][CH2:11]1)=[O:5])[CH3:2]

参加物

6

反応物 3

HCID 6397ChlorotrimethylsilaneHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 178418339Butyllithium

生成物 1

HCID 133449251-Ethoxycarbonyl-4-trimethylsilylpiperazine

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

A solution of 20 g of 1-ethoxycarbonylpiperazine in 400 ml dry tetrahydrofuran is cooled to -65° and 61.5 ml of 2.1M solution of n-butyllithium in hexane is added dropwise over a period of 15 minutes. The mixture is stirred for 15 minutes and a solution of 16.44 ml of chlorotrimethylsilane in 68 ml of tetrahydrofuran is added dropwise over a period of 15 minutes. The mixture is then allowed to warm up to room temperature overnight and evaporated to dryness. Ethyl ether is added, the solids are filtered off, the filtrate is evaporated to dryness and the residue is distilled to give 1-ethoxycarbonyl-4-trimethylsilylpiperazine, b.p. 102°-107°/0.1 mm/Hg.

後処理

  1. customevaporated to dryness
  2. additionEthyl ether is added
  3. filtrationthe solids are filtered off
  4. customthe filtrate is evaporated to dryness
  5. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-3226008c2cca414e8003e352912c1b3f
出典データセット
uspto-grants-1984_07
特許番号
US04460587

反応ノート

読み込み中…