2,4,6-Trimethylaniline → HCID 10537962, 화합물

HRID 1884337노트

반응식

HRID 1884337 반응식
Br[CH2:2][C:3](=[C:5]([C:8]#[N:9])[C:6]#[N:7])[CH3:4].[CH3:10][C:11]1[CH:17]=[C:16]([CH3:18])[CH:15]=[C:14]([CH3:19])[C:12]=1[NH2:13]>C(O)(C)C>[NH2:7][C:6]1[N:13]([C:12]2[C:14]([CH3:19])=[CH:15][C:16]([CH3:18])=[CH:17][C:11]=2[CH3:10])[CH:2]=[C:3]([CH3:4])[C:5]=1[C:8]#[N:9]

참가 물질

4

반응물 2

HCID 69132,4,6-TrimethylanilineHCID 10921206HCID 10921206, 화합물

생성물 1

HCID 10537962HCID 10537962, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture 2-(2-bromo-1-methyl-ethyl idene)-malononitrile and 2,4,6-trimethylaniline (17.330 g, 91.24 mmol) in 40 mL of isopropanol was stirred at room temperature for 15 hours. The reaction mixture was concentrated to dryness and diluted with chloroform and water. The chloroform layer was neutralized with dilute sodium hydroxide and washed with brine, separated, dried and concentrated to give 33.000 g of brown oily solid. The solid was purified through silica gel column chromatography to give 9.35 g (47.5%) of the title compound as an orange-yellow solid. 1H NMR (CDCl3) δ 2.0(s, 6H), 2.15(s, 3H), 2.35(s, 3H), 3.75(brs, 2H), 5.8(s, 1H), 6.95(s, 2H) ppm.

후처리

  1. concentrationThe reaction mixture was concentrated to dryness
  2. additiondiluted with chloroform and water
  3. washwashed with brine
  4. customseparated
  5. customdried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-5bfd974caf0b4150b545c7360deea656
출처 데이터셋
uspto-grants-2004_07
특허 번호
US06765008B1

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