Lithium Hydroxide → HCID 67494522、化合物

HRID 2047047ノート

反応式

HRID 2047047 の反応式
[NH2:1][C:2]1[N:7]2[N:8]=[CH:9][C:10]([C:11]3[CH:12]=[N:13][C:14]4[C:19]([CH:20]=3)=[CH:18][CH:17]=[CH:16][CH:15]=4)=[C:6]2[N:5]=[C:4]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][C:29]([O:31]C)=[O:30])=[CH:24][CH:23]=2)[C:3]=1[Br:33].[Li+].[OH-]>C1COCC1>[NH2:1][C:2]1[N:7]2[N:8]=[CH:9][C:10]([C:11]3[CH:12]=[N:13][C:14]4[C:19]([CH:20]=3)=[CH:18][CH:17]=[CH:16][CH:15]=4)=[C:6]2[N:5]=[C:4]([CH2:21][C:22]2[CH:27]=[CH:26][C:25]([CH2:28][C:29]([OH:31])=[O:30])=[CH:24][CH:23]=2)[C:3]=1[Br:33]

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 66735636HCID 66735636、化合物

生成物 1

HCID 67494522HCID 67494522、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Crude Methyl 2-(4-((7-amino-6-bromo-3-(quinolin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)methyl)phenyl)acetate from step F was dissolved in THF (5 mL) and LiOH (1N, 1 mL) was added. The mixture was stirred at room temperature overnight. The solvent was removed under vacuo, and the resulting residue was taken over with water and the pH value was adjusted to 5˜6. The solid was collected with filtration and purified with HPLC gave the product 2-(4-((7-amino-6-bromo-3-(quinolin-3-yl)pyrazolo[1,5-a]pyrimidin-5-yl)methyl)phenyl)acetic acid. HPLC-MS tR=1.53 min (UV254 nm); mass calculated for formula C24H18BrN5O2 487.1, observed LCMS m/z 487.9 (M+H).

後処理

  1. customThe solvent was removed under vacuo
  2. filtrationThe solid was collected with filtration
  3. custompurified with HPLC

出典と根拠

ORDレコード
ord-b2197a36b1624a9b98da22339db04b77
出典データセット
uspto-grants-2013_11
特許番号
US08591943B2

反応ノート

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