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Water → 4-(4-Fluorophenyl)-7-(morpholin-4-ylmethyl)quinoline-2-carboxamide

HRID 922770
ノート
印刷プレビュー

反応式

HRID 922770 の反応式
Br[CH2:2][C:3]1[CH:12]=[C:11]2[C:6]([C:7]([C:15]3[CH:20]=[CH:19][C:18]([F:21])=[CH:17][CH:16]=3)=[CH:8][C:9]([C:13]#[N:14])=[N:10]2)=[CH:5][CH:4]=1.[NH:22]1[CH2:27][CH2:26][O:25][CH2:24][CH2:23]1.[OH-:28].[Na+].O>C(#N)C>[F:21][C:18]1[CH:19]=[CH:20][C:15]([C:7]2[C:6]3[C:11](=[CH:12][C:3]([CH2:2][N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)=[CH:4][CH:5]=3)[N:10]=[C:9]([C:13]([NH2:14])=[O:28])[CH:8]=2)=[CH:16][CH:17]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8083MorpholineHCID 14798Sodium HydroxideHCID 194270117-(Bromomethyl)-4-(4-fluorophenyl)quinoline-2-carbonitrile

生成物 1

HCID 895451894-(4-Fluorophenyl)-7-(morpholin-4-ylmethyl)quinoline-2-carboxamide収率 89%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

反応条件

温度
50 °C

実験手順

To a room temperature solution of 7-(bromomethyl)-4-(4-fluorophenyl)quinoline-2-carbonitrile (2-1, 311.0 mg, 0.895 mmol, 1.0 equiv.) in acetonitrile (10.0 mL) was added morphline (85.77 mg, 0.985 mmol, 1.1 equiv.) and 5.0 M aqueous NaOH (2.69 mL, 13.43 mmol, 15 equiv.), and the resulting mixture was stirred at 50° C. for 4 days. After cooling to room temperature, water (100.0 mL) was added and the mixture was stirred for 30 minutes. A yellow solid was collected via suction filtration, washed with water, dried in vacuo. The solid was purified by reverse phase HPLC (H2O/CH3CN gradient w/0.1% TFA modifier) to afford 4-(4-fluorophenyl)-7-(morpholin-4-ylmethyl)quinoline-2-carboxamide (4-1, 291.0 mg, 80.0%) as a colorless solid. 1H NMR (500 MHz, CDCl3): δ 8.216 (s, 1H); 8.098 (br s, 2H); 7.911 (d, J=8.54 Hz, 1H); 7.642 (d, J=8.55 Hz, 1H); 7.503-7.529 (m, 2H); 7.219-7.263 (m, 2H); 5.798 (br s, 1H); 3.734 (br s, 6H); 2.528 (br s, 2H). LRMS m/z (M+H)+ 366.2 found, 366.2 required.

後処理

  1. temperatureAfter cooling to room temperature
  2. stirringthe mixture was stirred for 30 minutes
  3. filtrationA yellow solid was collected via suction filtration
  4. washwashed with water
  5. customdried in vacuo
  6. customThe solid was purified by reverse phase HPLC (H2O/CH3CN gradient w/0.1% TFA modifier)

出典と根拠

ORDレコード
ord-f1b8ad40176646839dfd377f439b5813
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278960B2

反応ノート

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