Chlorotrimethylsilane → 1-Ethoxycarbonyl-4-trimethylsilylpiperazine

HRID 1462177ノート

反応式

HRID 1462177 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 was cooled to -65° and 61.5 ml of 2.1M solution of n-butyllithium in hexane was added dropwise over a period of 15 minutes. The mixture was stirred for 15 minutes and a solution of 16.44 ml of chlorotrimethylsilane in 68 ml of tetrahydrofuran was added dropwise over a period of 15 minutes. The mixture was then allowed to warm up to room temperature overnight and evaporated to dryness. Ethyl ether was added, the solids were filtered off, the filtrate was evaporated to dryness and the residue was 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 was added
  3. filtrationthe solids were filtered off
  4. customthe filtrate was evaporated to dryness
  5. distillationthe residue was distilled

出典と根拠

ORDレコード
ord-71300a2896b040ccaed719785e66a580
出典データセット
uspto-grants-1984_07
特許番号
US04459232

反応ノート

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