Morpholine → 4-Morpholino-2-nitrobenzonitrile

HRID 1431245

反応式

HRID 1431245 の反応式
Cl[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=1.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1>C1COCC1>[O:16]1[CH2:17][CH2:18][N:13]([C:2]2[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[C:4]([N+:10]([O-:12])=[O:11])[CH:3]=2)[CH2:14][CH2:15]1

参加物

4

反応物 2

HCID 8083MorpholineHCID 969244-Chloro-2-nitrobenzonitrile

生成物 1

HCID 134992654-Morpholino-2-nitrobenzonitrile

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 4-chloro-2-nitrobenzonitrile (2.0 g, 11 mmol) in THF (40 mL) was added morpholine (1.0 g, 11 mmol). The reaction was heated at reflux overnight. After this time the reaction was cooled to rt and then it was partitioned between EtOAc (150 mL) and NaHCO3 (50 mL, satd aq. solution). The separated organic layer was dried over magnesium sulfate, filtered and evaporated in vacuo. Column chromatography (hexanes:EtOAc, 1:0 to 1:1) gave 4-morpholino-2-nitrobenzonitrile.

後処理

  1. temperatureThe reaction was heated
  2. temperatureat reflux overnight
  3. customit was partitioned between EtOAc (150 mL) and NaHCO3 (50 mL, satd aq. solution)
  4. dry with materialThe separated organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-9b10deb16b3e47efb2cf95c1b8f87c24
出典データセット
uspto-grants-2015_01
特許番号
US08940724B2

関連ノート

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