Morpholine → 4-Morpholino-2-nitrobenzonitrile

HRID 1431245

반응식

HRID 1431245 반응식
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

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 969244-Chloro-2-nitrobenzonitrile

생성물 1

HCID 134992654-Morpholino-2-nitrobenzonitrile

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9b10deb16b3e47efb2cf95c1b8f87c24
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08940724B2

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