Lithium Hydroxide → HCID 57471876、化合物

HRID 558995ノート

反応式

HRID 558995 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH:19]=[CH:18][CH:17]=[N:16]3)=[C:11]([F:20])[CH:10]=2)[C:5]([C:21]([O:23]CC)=[O:22])=[CH:4][N:3]=1.[Li+].[OH-]>C1COCC1>[Cl:1][C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([N:15]3[CH:19]=[CH:18][CH:17]=[N:16]3)=[C:11]([F:20])[CH:10]=2)[C:5]([C:21]([OH:23])=[O:22])=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 59199531HCID 59199531、化合物

生成物 1

HCID 57471876HCID 57471876、化合物収率 90.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 2-chloro-4-(3-fluoro-4-(1H-pyrazol-1-yl)phenylamino)pyrimidine-5-carboxylate (275 mg, 0.761 mmol) in THF (4 mL), aq. 1N LiOH (1.25 mL, 1.25 mmol) was added. The mixture was stirred at room temperature overnight. Upon acidification of the mixture with 1N HCl, white solids precipitated out, which were collected, and dried on vacuum to give 2-chloro-4-(3-fluoro-4-(1H-pyrazol-1-yl)phenylamino)pyrimidine-5-carboxylic acid (230 mg). MS 334.3 and 336.3 (M+H, Cl pattern)

後処理

  1. customUpon acidification of the mixture with 1N HCl, white solids precipitated out
  2. customwhich were collected
  3. customdried on vacuum

出典と根拠

ORDレコード
ord-c29ede0e368f44b6b23452dadfe7d12e
出典データセット
uspto-grants-2011_11
特許番号
US08063058B2

反応ノート

読み込み中…