Lithium Hydroxide → HCID 58098843、化合物

HRID 384278

反応式

HRID 384278 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][N:13]([CH3:15])[CH:14]=2)[C:5]([C:16]([O:18]CC)=[O:17])=[CH:4][N:3]=1.[Li+].[OH-]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][CH2:9][C:10]2[CH:11]=[N:12][N:13]([CH3:15])[CH:14]=2)[C:5]([C:16]([OH:18])=[O:17])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 58098673ethyl 2-chloro-4-((1-methyl-1H-pyrazol-4-yl)methylamino)pyrimidine-5-carboxylate

生成物 1

HCID 58098843HCID 58098843、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of give ethyl 2-chloro-4-((1-methyl-1H-pyrazol-4-yl)methylamino)pyrimidine-5-carboxylate (crude from step 1) in THF (9 mL), aq. 1N LiOH (6.6 mL, 6.6 mmol) was added. The mixture was stirred at room temperature overnight. THF was removed under vacuum, and the residue was acidified of with 1N HCl, the precipitated white solids were collected, and dried on vacuum to give 2-chloro-4-((1-methyl-1H-pyrazol-4-yl)methylamino)pyrimidine-5-carboxylic acid (1 g). MS 268.2, 270.2 (M+H, Cl pattern).

後処理

  1. customTHF was removed under vacuum
  2. customthe precipitated white solids were collected
  3. customdried on vacuum

出典と根拠

ORDレコード
ord-0a5b6b485ef34f12addd0eadd17fd7f7
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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