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Hydrochloric Acid → [Allyl-(5,6-dichloro-pyridin-3-yl)-amino]-acetaldehyde

HRID 898738
ノート
印刷プレビュー

反応式

HRID 898738 の反応式
[CH2:1]([N:4]([C:11]1[CH:12]=[N:13][C:14]([Cl:18])=[C:15]([Cl:17])[CH:16]=1)[CH2:5][CH:6](OC)[O:7]C)[CH:2]=[CH2:3].Cl.ClCCl>O1CCCC1.O>[CH2:1]([N:4]([CH2:5][CH:6]=[O:7])[C:11]1[CH:12]=[N:13][C:14]([Cl:18])=[C:15]([Cl:17])[CH:16]=1)[CH:2]=[CH2:3]
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

6

反応物 3

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 57448418Allyl-(5,6-dichloro-pyridin-3-yl)-(2,2-dimethoxy-ethyl)amine

生成物 1

HCID 57448419[Allyl-(5,6-dichloro-pyridin-3-yl)-amino]-acetaldehyde

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran
溶媒

反応条件

温度
15 °C

実験手順

A solution of allyl-(5,6-dichloro-pyridin-3-yl)-(2,2-dimethoxy-ethyl)-amine (57.2 g) in tetrahydrofuran (443 g) was cooled to 10° C. A solution of concentrated hydrochloric acid (136 g) in water (114 g) was slowly added, maintaining the temperature below 20° C. The reaction was then stirred at 15° C. for about 4 hours. Then dichloromethane (570 g) and water (430 g) were added and the layers separated. The organic layer was washed with 5% aqueous sodium bicarbonate (453 g), and then washed twice with water (430 g). The organic layer was concentrated and the residue dissolved in dichloromethane (580 g).

後処理

  1. temperaturemaintaining the temperature below 20° C
  2. customthe layers separated
  3. washThe organic layer was washed with 5% aqueous sodium bicarbonate (453 g)
  4. washwashed twice with water (430 g)
  5. concentrationThe organic layer was concentrated
  6. dissolutionthe residue dissolved in dichloromethane (580 g)

出典と根拠

ORDレコード
ord-a9ed1b4d10ec401c81c965c23b6b8bf1
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07351833B2

反応ノート

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