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

HRID 2054890

反応式

HRID 2054890 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f2505ceb71034e728e2a4655b9a619a7
出典データセット
uspto-grants-2008_02
特許番号
US07329764B2

関連ノート

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