D-Tartaric acid → (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate

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:44])(=[O:43])[C@H:36]([C@@H:38]([C:40]([OH:42])=[O:41])[OH:39])[OH:37]>>[C:40]([C@H:38]([C@@H:36]([C:35]([OH:44])=[O:43])[OH:37])[OH:39])([OH:42])=[O:41].[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

反応物 2

HCID 439655D-Tartaric acid

HCID 25262965Azd8055

生成物 1

HCID 69031901(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate

実験手順

(5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol (1.50 g (96% w/w, 3.1 mmoles), D-tartaric Acid (0.51 g, 3.4 mmoles) and methylated spirit industrial 74 O.P. (15.0 ml) were charged to a 100 ml reactor and heated to reflux. Product began to precipitate. On cooling more product precipitated. Product was isolated, washed with methylated spirit industrial 74 O.P. and dried in vacuum oven at 50 C for 4 h to yield 1.98 g of (5-{2,4-Bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol D-Tartrate as a yellow solid.

後処理

addition(15.0 ml) were charged to a 100 ml reactor
temperatureheated to reflux
customto precipitate
temperatureOn cooling more product
customprecipitated
customProduct was isolated
washwashed with methylated spirit industrial 74 O.P
customand dried in vacuum oven at 50 C for 4 h

出典と根拠

ORDレコード: ord-4e1ed4ceb435415093405d316ac36221
出典データセット: uspto-grants-2012_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08198441B2

反応ノート

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