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Ammonia → HCID 54355418、化合物

HRID 2286712
ノート
印刷プレビュー

反応式

HRID 2286712 の反応式
[NH2-:1].[Na+].[NH3:3].[CH3:4][N:5]([CH3:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH3:13][CH2:14][CH2:15][CH2:16][CH:17]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[CH2:18][CH2:19][CH2:20][CH3:21].[H][H]>[Fe].O>[CH3:13][CH2:14][CH2:15][CH2:16][CH:17]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[CH2:18][CH2:19][CH2:20][CH3:21].[NH2:1][C:4]1[C:22]([CH:17]([CH2:16][CH2:15][CH2:14][CH3:13])[CH2:18][CH2:19][CH2:20][CH3:21])=[CH:27][CH:26]=[CH:25][N:3]=1.[CH3:13][CH2:14][CH2:15][CH2:16][CH:17]([C:22]1[N:23]=[C:24]([C:7]2[CH:15]=[CH:14][CH:13]=[C:9]([CH:10]([CH2:11][CH2:6][CH2:5][CH3:12])[CH2:16][CH2:17][CH2:18][CH3:19])[N:8]=2)[CH:25]=[CH:26][CH:27]=1)[CH2:18][CH2:19][CH2:20][CH3:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 222Ammonia2 回HCID 949N,N-DimethylanilineHCID 24533Sodium amideHCID 137778Pyridine, 2-(1-butylpentyl)-HCID 178418361HCID 178418361、化合物2 回

生成物 3

HCID 137778Pyridine, 2-(1-butylpentyl)-
HCID 23462093
2-(Nonan-5-yl)-6-[6-(nonan-5-yl)pyridin-2-yl]pyridine
HCID 54355418HCID 54355418、化合物収率 2.7%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 962Water溶媒

反応条件

温度
152 °C

実験手順

In a two-liter, three-neck flask, equipped with a stirrer and dropping funnel, was prepared 0.20 mole of sodamide, using an iron catalyst, in about 600 cc of liquid ammonia. The ammonia was replaced by adding 1,000 g of N,N-dimethylaniline through the dropping funnel and evaporating the ammonia. A thermometer and reflux condenser were added to the flask. The mixture was heated to 152° C. and 205 g (1.0 mole) of 2-(5-nonyl)pyridine was added. No reaction took place. The mixture was slowly heated to 197° C. when hydrogen evolution started, and the reaction mixture turned purple. The reaction continued at 197°-198° C. for 3 hours, at which time the hydrogen evolution became slow. The reaction mixture was cooled to about room temperature and hydrolyzed with 200 cc of water. The oil layer was separated and distilled to give 125 g (0.61 mole) of unreacted 2-(5-nonyl)pyridine, B 2.3 g (0.01 mole) of 2-amino-(5-nonyl)pyridine (2.7% yield) and 35.8 g (0.09 mole) of 6,6'-di-(5-nonyl)-2,2'-bipyridyl boiling at 251°-259° C. and 7 mm Hg. The yield of 2,2'-bipyridyl product based on recovered 2-(5-nonyl)pyridine was 45.0%.

後処理

  1. customIn a two-liter, three-neck flask, equipped with a stirrer
  2. customevaporating the ammonia
  3. temperatureA thermometer and reflux condenser
  4. additionwere added to the flask
  5. customThe oil layer was separated
  6. distillationdistilled

出典と根拠

ORDレコード
ord-9d226b7475ab4156a806f5a0cfaba462
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04267335

反応ノート

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