5-chloro-2,2-dimethylpentanenitrile → 3,4,5,6-Tetrahydro-2,3,3-trimethylpyridine

HRID 1577291노트

반응식

HRID 1577291 반응식
[CH3:1][Li].Cl[CH2:4][CH2:5][CH2:6][C:7]([CH3:11])([CH3:10])[C:8]#[N:9]>CCOCC>[CH3:1][C:8]1[C:7]([CH3:11])([CH3:10])[CH2:6][CH2:5][CH2:4][N:9]=1

참가 물질

4

반응물 2

HCID 2642175-chloro-2,2-dimethylpentanenitrileHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 131577763,4,5,6-Tetrahydro-2,3,3-trimethylpyridine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

0.1 mol of methyl lithium dissolved in 200 ml of ether anhydride is added drop by drop in an inert atmosphere (argon or nitrogen) to 15 g of 5-chloro-2,2-dimethyl pentane nitrile diluted in 60 ml of anhydrous ether. The reaction mixture is maintained between 0° and 5° C. during the addition and then for a further 30 minutes and then kept at room temperature for 4 hours. After hydrolysis it is extracted with ether. The 2,3,3-trimethyl-3,4,5,6-tetrahydropyridine is then isolated by distillation. A colorless liquid of B.P.14 =60° C. is obtained in a yield of 76% of 1-piperideine.

후처리

  1. temperatureThe reaction mixture is maintained between 0° and 5° C. during the addition
  2. waitkept at room temperature for 4 hours
  3. customAfter hydrolysis it
  4. extractionis extracted with ether

출처 및 근거

ORD 기록
ord-5cf60033b1114b4991f12c32ea544805
출처 데이터셋
uspto-grants-1981_09
특허 번호
US04287337

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