Ethyl 2-(methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylate → 2-(Methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylic acid

HRID 533474

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>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

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 LiOHH2O (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

customTHF was removed under vacuum
customprecipitated out
filtrationwhich were collected by filtration
customdried on vacuum

出典と根拠

ORDレコード: ord-be23b1820d3f489a97e26d40e4f451d1
出典データセット: uspto-grants-2014_10
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08853230B2

反応式

参加物

反応物 1

生成物 1

試薬・触媒・溶媒 2

実験手順

後処理

出典と根拠

関連ノート