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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Toluene → 1-(N,N-dimethylamino)-2,3-dicyanoprop-1-ene

HRID 1720463
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HRID 1720463 반응식
[K].O[CH:3]=[C:4]([C:8]#[N:9])[CH2:5][C:6]#[N:7].C1(C)C=CC=CC=1.Cl.[CH3:18][NH:19][CH3:20]>CN(C=O)C>[CH3:18][N:19]([CH:3]=[C:4]([C:8]#[N:9])[CH2:5][C:6]#[N:7])[CH3:20]
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참가 물질

6

반응물 4

HCID 1140TolueneHCID 10473Dimethylamine, hydrochlorideHCID 5462222PotassiumHCID 727412321,2-Dicyano-3-hydroxyprop-2-ene

생성물 1

HCID 537608131-(N,N-dimethylamino)-2,3-dicyanoprop-1-ene수율 86%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A 12 liter three-necked round-bottomed flask, fitted with a mechanical stirrer, water condenser, nitrogen inlet and bubbler, was charged with 877 g (6 moles) of the potassium salt of 1-hydroxy-2,3-dicyanoprop-1-ene in 61 of anhydrous toluene and 300 ml of anhydrous DMF. To this heterogeneous mixture was added 514 g (6.3 moles) of dimethylamine hydrochloride. The mixture was heated to 80° then cooled to room temperature, filtered and the filter cake rinsed with toluene. The filtrate was concentrated under vacuum to yield 933 g containing on 75% weight, 86% yield of an off which partially crystallized at -5° C. An aliquot of the crystalline portion was collected and recrystallized twice from ether to give white crystals, m.p. 49° C. of 1-(N,N-dimethylamino)-2,3-dicyanoprop-1-ene (CIS 1).

후처리

  1. customA 12 liter three-necked round-bottomed flask, fitted with a mechanical stirrer, water condenser, nitrogen inlet
  2. temperatureThe mixture was heated to 80°
  3. filtrationfiltered
  4. washthe filter cake rinsed with toluene
  5. concentrationThe filtrate was concentrated under vacuum
  6. customto yield 933 g
  7. additioncontaining on 75% weight, 86% yield of an off which
  8. custompartially crystallized at -5° C
  9. customAn aliquot of the crystalline portion was collected
  10. customrecrystallized twice from ether

출처 및 근거

ORD 기록
ord-d16122fa10994e959be8d12cb080d1b3
출처 데이터셋
uspto-grants-1996_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05506260

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