Chlorotrimethylsilane → 1-Ethoxycarbonyl-4-trimethylsilylpiperazine

HRID 1462177노트

반응식

HRID 1462177 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 133449251-Ethoxycarbonyl-4-trimethylsilylpiperazine

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-71300a2896b040ccaed719785e66a580
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04459232

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