Lithium hydroxide, monohydrate → 2-(Methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylic acid

HRID 384270

反応式

HRID 384270 の反応式
[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:12][CH2:11]2)[C:6]([C:19]([O:21]CC)=[O:20])=[CH:5][N:4]=1.O[Li].O>C1COCC1.O>[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:11][CH2:12]2)[C:6]([C:19]([OH:21])=[O:20])=[CH:5][N:4]=1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 58098733Ethyl 2-(methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylate

生成物 1

HCID 580987872-(Methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 2-(methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylate (crude from step 2) in THF (4 mL) was added LiOH.H2O (150 mg, 3.57 mmol) in H2O (2 mL). The mixture was stirred at room temperature overnight. THF was removed under vacuum and the residue was acidified with 1N HCl, white solids precipitated out, which were collected by filtration, dried on vacuum to give 2-(methylthio)-4-(1-phenylcyclopropylamino) pyrimidine-5-carboxylic acid (646 mg). MS 302.3 (M+H).

後処理

  1. customTHF was removed under vacuum
  2. customprecipitated out
  3. filtrationwhich were collected by filtration
  4. customdried on vacuum

出典と根拠

ORDレコード
ord-469f60f002e24906ace889bfbaca4df7
出典データセット
uspto-grants-2013_02
特許番号
US08367689B2

関連ノート

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