Dichloromethane → HCID 86699684、化合物

HRID 1487192

反応式

HRID 1487192 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]([N+:13]([O-:15])=[O:14])=[C:6]([CH:8]2[O:12][CH2:11][CH2:10][O:9]2)[CH:7]=1.ClCCl.[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1>>[O:9]1[CH2:10][CH2:11][O:12][CH:8]1[C:6]1[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[CH:3]=[CH:4][C:5]=1[N+:13]([O-:15])=[O:14]

参加物

4

反応物 3

HCID 6344DichloromethaneHCID 8083MorpholineHCID 2673852-(5-Chloro-2-nitrophenyl)-1,3-dioxolane

生成物 1

HCID 86699684HCID 86699684、化合物収率 97.1%

実験手順

2-(5-Chloro-2-nitrophenyl)-1,3-dioxolane (13.4 g, 58.4 mmol) was dissolved in morpholine (150 mL). The mixture was then heated to reflux for 16 hours. Cooling to room temperature, dichloromethane was added. The organic phase was washed with water, dried over anhydrous sodium sulfate, evaporated and purified by silica gel chromatography to afford the product 4-(3-(1,3-dioxolan-2-yl)-4-nitrophenyl)morpholine (15.9 g, yield 97.1%).

後処理

  1. temperatureThe mixture was then heated
  2. temperatureto reflux for 16 hours
  3. washThe organic phase was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customevaporated
  6. custompurified by silica gel chromatography

出典と根拠

ORDレコード
ord-4a084a21f93a422d9e51761a639bc4a8
出典データセット
uspto-grants-2016_08
特許番号
US09428508B2

関連ノート

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