Fumaric Acid → AZD-8055 fumarate

HRID 218357ノート

反応式

HRID 218357 の反応式
[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1.[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39]>O>[C:35]([OH:42])(=[O:41])/[CH:36]=[CH:37]/[C:38]([OH:40])=[O:39].[CH3:1][C@H:2]1[CH2:7][O:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[C:10]([N:28]2[CH2:33][CH2:32][O:31][CH2:30][C@@H:29]2[CH3:34])[C:11]2[CH:17]=[CH:16][C:15]([C:18]3[CH:19]=[CH:20][C:21]([O:26][CH3:27])=[C:22]([CH2:24][OH:25])[CH:23]=3)=[N:14][C:12]=2[N:13]=1

参加物

4

反応物 2

HCID 444972Fumaric AcidHCID 25262965Azd8055

生成物 1

HCID 44537932AZD-8055 fumarate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
92 °C

実験手順

(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol (10.00 g (96% w/w, 20.6 moles), fumaric Acid (2.63 g, 22.7 mmoles), water (84 ml) and methylated spirit industrial 74 O.P. (16.0 ml) were charged to a 250 ml reactor and heated to reflux (92° C.). The hot solution was filtered to remove extraneous matter. The filter was washed with a mixture of water (17 ml and methylated spirit industrial 74 O.P. (3 ml). On cooling the combined filtrates product precipitated. Product was isolated, washed with methylated spirit industrial 74 O.P. and dried to yield 10.12 g of (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol Fumarate as a yellow solid.

後処理

  1. addition(16.0 ml) were charged to a 250 ml reactor
  2. temperatureheated
  3. filtrationThe hot solution was filtered
  4. customto remove extraneous matter
  5. washThe filter was washed with a mixture of water (17 ml and methylated spirit industrial 74 O.P
  6. temperatureOn cooling the combined filtrates product
  7. customprecipitated
  8. customProduct was isolated
  9. washwashed with methylated spirit industrial 74 O.P
  10. customand dried

出典と根拠

ORDレコード
ord-8cc3de73fb3845a8ac8267a46faf47d1
出典データセット
uspto-grants-2012_06
特許番号
US08198441B2

反応ノート

読み込み中…