Lithium Hydroxide → HCID 67494522, 화합물

HRID 2047047노트

반응식

HRID 2047047 반응식
[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]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 66735636HCID 66735636, 화합물

생성물 1

HCID 67494522HCID 67494522, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-b2197a36b1624a9b98da22339db04b77
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08591943B2

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