2,4,6-Trimethylaniline → HCID 10537962、化合物

HRID 1884337ノート

反応式

HRID 1884337 の反応式
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]

参加物

4

反応物 2

HCID 69132,4,6-TrimethylanilineHCID 10921206HCID 10921206、化合物

生成物 1

HCID 10537962HCID 10537962、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-5bfd974caf0b4150b545c7360deea656
出典データセット
uspto-grants-2004_07
特許番号
US06765008B1

反応ノート

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