Morpholine → 4-(Morpholin-4-yl)benzamide

HRID 2120266ノート

反応式

HRID 2120266 の反応式
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.F[C:8]1[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[O:13])=[CH:10][CH:9]=1>O>[N:1]1([C:8]2[CH:16]=[CH:15][C:11]([C:12]([NH2:14])=[O:13])=[CH:10][CH:9]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

参加物

4

反応物 2

HCID 8083MorpholineHCID 715724-Fluorobenzamide2 回

生成物 1

HCID 221422424-(Morpholin-4-yl)benzamide収率 3,373%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
120 °C

実験手順

A mixture of morpholine (2.0 g, 0.23 mmol) and 4-fluorobenzamide (1.2 g, 8.6 mmol) is heated at 120° C. The conversion of the 4-fluorobenzoamide is complete after 10 hours. Water (10 ml) is than added into the reaction mixture. The precipitate is filtered off, washed with water and dried under vacuum (30° C.) to give 1.6 g of the title-compound. Yield: 94%; m.p. 220-221° C.; MS 206 (100, M+); H1 NMR (DMSO): δ 7.76 (d, 2H), 7.75 (b, 1H), 7.05 (b, 1H), 6.94 (d, 21H), 3.73 (t, 4H), 3.20 (t, 4H); C13 NMR (CDCl3): δ 167.61, 152.90, 128.79, 123.93, 113.31, 65.92, 47.36.

後処理

  1. additionthan added into the reaction mixture
  2. filtrationThe precipitate is filtered off
  3. washwashed with water
  4. customdried under vacuum (30° C.)

出典と根拠

ORDレコード
ord-970cc2e649334d5dba348895f698a763
出典データセット
uspto-grants-2004_02
特許番号
US06689882B2

反応ノート

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