Morpholine → 2,6-Difluoro-4-(morpholin-4-yl)benzonitrile

HRID 2054890

반응식

HRID 2054890 반응식
[F:1][C:2]1[CH:9]=[C:8](F)[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5].[NH:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1.C(N(CC)C(C)C)(C)C>CO.O>[F:1][C:2]1[CH:9]=[C:8]([N:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)[CH:7]=[C:6]([F:11])[C:3]=1[C:4]#[N:5]

참가 물질

6

반응물 3

HCID 8083MorpholineHCID 81531DiisopropylethylamineHCID 7371772,4,6-Trifluorobenzonitrile

생성물 1

HCID 115286822,6-Difluoro-4-(morpholin-4-yl)benzonitrile수율 68.6%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

To a solution of 1.0 g (6.37 mmol) of 2,4,6-trifluorobenzonitrile in MeOH (25 mL) was added 0.6 mL (6.9 mmol) of morpholine and 1.2 mL (6.7 mmol) of N,N-diisopropylethylamine. The mixture was heated to 50° C. for 6 h then cooled to room temperature and diluted with H2O which caused a solid to precipitate from solution. The white solid was collected by filtration, washed with H2O and dried under vacuum to provide 0.98 g (68%) of 2,6-difluoro-4-morpholin-4-yl-benzonitrile as a white solid.

후처리

  1. temperaturethen cooled to room temperature
  2. customto precipitate from solution
  3. filtrationThe white solid was collected by filtration
  4. washwashed with H2O
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-f2505ceb71034e728e2a4655b9a619a7
출처 데이터셋
uspto-grants-2008_02
특허 번호
US07329764B2

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