反応式
[NH2:1][C:2]1[N:7]=[C:6]([S:8][CH:9]([C:11]2[CH:12]=[C:13]([C:17]([O:19]C)=[O:18])[CH:14]=[CH:15][CH:16]=2)[CH3:10])[C:5]([C:21]#[N:22])=[C:4]([C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][O:32][CH3:33])=[CH:25][CH:24]=2)[C:3]=1[C:34]#[N:35].[OH-].[Li+].Cl>O1CCCC1>[NH2:1][C:2]1[N:7]=[C:6]([S:8][CH:9]([C:11]2[CH:12]=[C:13]([C:17]([OH:19])=[O:18])[CH:14]=[CH:15][CH:16]=2)[CH3:10])[C:5]([C:21]#[N:22])=[C:4]([C:23]2[CH:28]=[CH:27][C:26]([O:29][CH2:30][CH2:31][O:32][CH3:33])=[CH:25][CH:24]=2)[C:3]=1[C:34]#[N:35]参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
150 mg (0.307 mmol) of methyl 3-[1-({6-amino-3,5-dicyano-4-[4-(2-methoxyethoxy)phenyl]-pyridin-2-yl}sulfanyl)ethyl]benzenecarboxylate (Example 65A) were dissolved in 7 ml of tetrahydrofuran. After addition of 14.7 mg (0.61 mmol) of lithium hydroxide, the mixture was stirred at RT overnight. The mixture was then stirred at 40° C. for 4 h. Using 1N hydrochloric acid, the pH of the reaction solution was adjusted to pH 4, and the clear solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid).
後処理
- stirringThe mixture was then stirred at 40° C. for 4 h
- customthe clear solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid)
出典と根拠
- ORDレコード
- ord-9be33fa4998242058e736580ee7a34c5
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09187428B2
関連ノート
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