Water → HCID 22291610、化合物

HRID 968111ノート

反応式

HRID 968111 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([NH:10][C:11]2[CH:33]=[CH:32][C:14]3[CH2:15][CH2:16][C:17]4[C:18]([C:29]([NH2:31])=[O:30])=[N:19][N:20]([C:22]5[CH:27]=[CH:26][C:25]([F:28])=[CH:24][CH:23]=5)[C:21]=4[C:13]=3[CH:12]=2)=[O:9])=[C:4]([CH3:34])[CH:3]=1.[NH:35]1[CH2:40][CH2:39][O:38][CH2:37][CH2:36]1.O>CN(C)C(=O)C>[F:28][C:25]1[CH:26]=[CH:27][C:22]([N:20]2[C:21]3[C:13]4[CH:12]=[C:11]([NH:10][C:8]([C:5]5[CH:6]=[N:7][C:2]([N:35]6[CH2:40][CH2:39][O:38][CH2:37][CH2:36]6)=[CH:3][C:4]=5[CH3:34])=[O:9])[CH:33]=[CH:32][C:14]=4[CH2:15][CH2:16][C:17]=3[C:18]([C:29]([NH2:31])=[O:30])=[N:19]2)=[CH:23][CH:24]=1

参加物

5

反応物 3

HCID 962WaterHCID 8083MorpholineHCID 22291445HCID 22291445、化合物

生成物 1

HCID 22291610HCID 22291610、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
100 °C

実験手順

The title compound of Example 246 (1.47 mmoles) and morpholine (23.1 mmoles) were dissolved in 10 mL of N,N-dimethylacetamide. The reaction mixture was then placed under nitrogen and stirred in an oil bath at 100° C. for 27 h. The mixture was partially stripped of solvent then added to water, filtered, and washed with water. The solid was recrystallized from acetonitrile, then dissolved in acetonitrile and dried over anhydrous MgSO4. The solvent was then stripped down to a solid. Mp: 301° C. (decomp.) 1H NMR (d6-DMSO, 400 MHz): δ 2.22 (s, 3H); 2.80-2.94 (m, 4H); 3.46 (t, 4H, J=4.8 Hz); 3.62 (t, 4H, J=4.8 Hz); 6.67 (s, 1H); 7.22-7.27 (m, 3H); 7.31-7.38 (m, 2H); 7.42 (dd, 1H, J=1.9 Hz, 8.2 Hz); 7.49-7.57 (m, 3H); 8.11 (s, 1H); 9.92 (s, 1H). 13C NMR (d6-DMSO, 100 MHz): δ 20.35, 20.38, 29.63, 45.55, 66.54, 108.46, 114.91, 117.02, 117.25, 119.91, 121.23, 122.78, 126.42, 128.64, 128.73, 129.36, 132.60, 136.82, 136.85, 138.38, 139.82, 143.15, 147.70, 148.03, 160.04, 161.39, 163.84, 164.47, 166.18. M+1=527

後処理

  1. filtrationfiltered
  2. washwashed with water
  3. customThe solid was recrystallized from acetonitrile
  4. dissolutiondissolved in acetonitrile
  5. dry with materialdried over anhydrous MgSO4

出典と根拠

ORDレコード
ord-3bf32bffc30140bebe1c802fa990437f
出典データセット
uspto-grants-2005_10
特許番号
US06956052B2

反応ノート

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