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Ethylenediamine → N-[2-(2-Methyl-1,3-dioxolan-2-yl)-4-pyridyl]ethane-1,2-diamine

HRID 333062
ノート
印刷プレビュー

反応式

HRID 333062 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2([CH3:13])[O:12][CH2:11][CH2:10][O:9]2)[CH:3]=1.[NH2:14][CH2:15][CH2:16][NH2:17]>>[CH3:13][C:8]1([C:4]2[CH:3]=[C:2]([NH:14][CH2:15][CH2:16][NH2:17])[CH:7]=[CH:6][N:5]=2)[O:12][CH2:11][CH2:10][O:9]1
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

3

反応物 2

HCID 3301EthylenediamineHCID 668355144-Chloro-2-(2-methyl-1,3-dioxolan-2-yl)pyridine

生成物 1

HCID 66835538N-[2-(2-Methyl-1,3-dioxolan-2-yl)-4-pyridyl]ethane-1,2-diamine収率 95.2%

反応条件

温度
180 °C

実験手順

4-Chloro-2-(2-methyl-1,3-dioxolan-2-yl)pyridine (500 mg, 2.5 mmol) was mixed with 1,2-diaminoethane (1.09 ml, 26.2 mmol) and stirred in a closed vessel at 180° C. with microwave heating for 30 minutes in two batches. The mixture was evaporated to dryness, the solid residue was washed with acetone. The washing solution was evaporated to dryness and this solid residue was washed with acetonitrile. The solid residues were combined and dried under reduced pressure to yield 531 mg of a solid (2.38 mmol, 95%). MS (APCI) m/z=224.1 [M+H]+.

後処理

  1. temperatureheating for 30 minutes in two batches
  2. customThe mixture was evaporated to dryness
  3. washthe solid residue was washed with acetone
  4. customThe washing solution was evaporated to dryness
  5. washthis solid residue was washed with acetonitrile
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-bec392ac1a5847c486292900401e513b
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08877934B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート