Chlorotrimethylsilane → 1-Ethoxycarbonyl-4-trimethylsilylpiperazine

HRID 1462444노트

반응식

HRID 1462444 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-3226008c2cca414e8003e352912c1b3f
출처 데이터셋
uspto-grants-1984_07
특허 번호
US04460587

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