Triethylamine → 9-Ethyl-3-(hydrazinylidenemethyl)-9H-carbazole

HRID 268575

反応式

HRID 268575 の反応式
O.[NH2:2][NH2:3].C(N(CC)CC)C.[CH2:11]([N:13]1[C:25]2[CH:24]=[CH:23][C:22]([CH:26]=O)=[CH:21][C:20]=2[C:19]2[C:14]1=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH3:12]>O1CCCC1.O>[CH2:11]([N:13]1[C:25]2[CH:24]=[CH:23][C:22]([CH:26]=[N:2][NH2:3])=[CH:21][C:20]=2[C:19]2[C:14]1=[CH:15][CH:16]=[CH:17][CH:18]=2)[CH3:12]

参加物

6

反応物 3

HCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 820559-ethyl-9H-carbazole-3-carbaldehyde

生成物 1

HCID 674839059-Ethyl-3-(hydrazinylidenemethyl)-9H-carbazole

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A quantity of 98% hydrazine monohydrate (50 ml, 1.4 mole, obtained from Aldrich, Milwaukee, Wis.) and 10 ml of triethylamine (obtained from Aldrich, Milwaukee, Wis.) were added to a 250 ml, 2-neck round bottom flask equipped with a mechanical stirrer and an addition funnel. The solution was stirred vigorously at room temperature for a period of 10-15 min. A solution of 9-ethyl-3-carbazolecarboxaldehyde (22.3 g, 0.1 mol, from Aldrich, Milwaukee, Wis.) in 30 ml of tetrahydrofuran (THF) were added slowly to the round bottom flask. After the addition of aldehyde was completed, the reaction mixture was stirred at room temperature for 2 hours. Next, the reaction mixture was diluted with 50 ml of water. A precipitate was collected by filtration and washed repeatedly with water to give crude 9-ethyl-3-carbazolecarboxaldehyde hydrazone, which was used in the next step immediately.

後処理

  1. customequipped with a mechanical stirrer and an addition funnel
  2. stirringthe reaction mixture was stirred at room temperature for 2 hours
  3. filtrationA precipitate was collected by filtration
  4. washwashed repeatedly with water

出典と根拠

ORDレコード
ord-e024a7e79af74dc399a5e20191e6eeff
出典データセット
uspto-grants-2008_11
特許番号
US07445877B2

関連ノート

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