4-tert-Butylcyclohexanone → 4-t-Butyl-2,2,6,6-tetra(beta-cyanoethyl)cyclohexanone

HRID 867045노트

반응식

HRID 867045 반응식
[C:1]([CH:5]1[CH2:10][CH2:9][C:8](=[O:11])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[K+].[C:14](#[N:17])[CH:15]=[CH2:16]>C(O)(C)(C)C>[C:1]([CH:5]1[CH2:6][C:7]([CH2:16][CH2:15][C:14]#[N:17])([CH2:16][CH2:15][C:14]#[N:17])[C:8](=[O:11])[C:9]([CH2:16][CH2:15][C:14]#[N:17])([CH2:16][CH2:15][C:14]#[N:17])[CH2:10]1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 73924-tert-ButylcyclohexanoneHCID 7855AcrylonitrileHCID 14797Potassium Hydroxide

생성물 1

HCID 203171724-t-Butyl-2,2,6,6-tetra(beta-cyanoethyl)cyclohexanone수율 75.2%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

A solution of 4-t-butylcyclohexanone (15.4g) and crushed KOH (0.5g) in tert.butanol (62.4g) was stirred and kept at or below 30° C. while acrylonitrile (21.2g) was added dropwise. During the addition a solid began to precipitate. When addition was complete the thick slurry was stirred for a further hour before the solid was collected by filtration. The solid was washed with water, then crystallised from 2-ethoxyethanol to yield 27.5g of 4-t-butyl-2,2,6,6-tetra(β-cyanoethyl)cyclohexanone, m.p. 175°-178° C.

후처리

  1. custombelow 30° C.
  2. additionwas added dropwise
  3. additionDuring the addition a solid
  4. customto precipitate
  5. additionWhen addition
  6. stirringwas stirred for a further hour before the solid
  7. filtrationwas collected by filtration
  8. washThe solid was washed with water
  9. customcrystallised from 2-ethoxyethanol

출처 및 근거

ORD 기록
ord-7007bf7277be499192aed1f994b6736b
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04102701

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