Lithium hydroxide, monohydrate → HCID 71571940, compound

HRID 589402Notes

Reaction equation

HRID 589402 reaction equation
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([NH:13][C:14]1[N:15]=[CH:16][C:17]([CH2:20][N:21]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]([CH2:30][C:31]([O:33]CC)=[O:32])=[N:22]2)=[N:18][CH:19]=1)=[O:12].O.[OH-].[Li+]>O1CCCC1>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([NH:13][C:14]1[N:15]=[CH:16][C:17]([CH2:20][N:21]2[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]([CH2:30][C:31]([OH:33])=[O:32])=[N:22]2)=[N:18][CH:19]=1)=[O:12]

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 89590272HCID 89590272, compound

Product 1

HCID 71571940HCID 71571940, compoundYield 29.7%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Ethyl 2-[1-[[5-(2-naphthamido)pyrazin-2-yl]methyl]-1H-indazol-3-yl]acetate (0.466 g, 1.0 mmol) was dissolved in 20 mL tetrahydrofuran, and in an ice bath, was added 10 mL aqueous solution dissolving lithium hydroxide monohydrate (0.18 g, 4.3 mmol). It was reacted at room temperature for 3 h, rotate evaporated to dryness to remove the solvent, purified by preparative liquid phase (methanol:water=50%) to obtain a white solid 130 mg, at a yield of 29.7%.

Workup

  1. customIt was reacted at room temperature for 3 h
  2. customrotate evaporated to dryness
  3. customto remove the solvent
  4. custompurified by preparative liquid phase (methanol:water=50%)

Sources & evidence

ORD record
ord-390dafe2ee404ebd8cc50c93a8502744
Source dataset
uspto-grants-2016_01
Patent number
US09233098B2

Reaction notes

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