Hydrochloride methanol → HCID 178461481, compound

HRID 2092096Notes

Reaction equation

HRID 2092096 reaction equation
[Cl:1][C:2]1[C:7](=[O:8])[N:6]([CH2:9][C:10]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][N:17]=[CH:16][CH:15]=2)=[O:11])[N:5]=[C:4]([O:20]COCC[Si](C)(C)C)[C:3]=1[NH:29][C@@H:30]1[CH2:35][C@@H:34]2[CH2:36][C@@H:32]([C:33]2([CH3:38])[CH3:37])[C@H:31]1[CH3:39].Cl.CO>CO>[ClH:1].[Cl:1][C:2]1[C:7](=[O:8])[N:6]([CH2:9][C:10]([NH:12][CH2:13][C:14]2[CH:15]=[CH:16][N:17]=[CH:18][CH:19]=2)=[O:11])[N:5]=[C:4]([OH:20])[C:3]=1[NH:29][C@@H:30]1[CH2:35][C@@H:34]2[CH2:36][C@@H:32]([C:33]2([CH3:38])[CH3:37])[C@H:31]1[CH3:39]

Participants

4

Reactant 2

HCID 21893726Hydrochloride methanolHCID 68431501HCID 68431501, compound

Product 1

HCID 178461481HCID 178461481, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

2-[5-Chloro-6-oxo-4-{[(1R,2R,3R,5S)-2,6,6-trimethylbicyclo[3.1.1]hept-3-yl]amino}-3-{[2-(trimethylsilyl)ethoxy]methoxy}pyridazin-1(6H)-yl]-N-(pyridin-4-ylmethyl)acetamide (12 mg, 0.0208 mmol) in methanol (1 mL) was stirred with 10 mass % hydrogen chloride-methanol (5 mL) at 60° C. for 5 hours. After completion of the reaction, the reaction solution was concentrated under reduced pressure and purified by preparative HPLC to give the desired product.

Workup

  1. customAfter completion of the reaction
  2. concentrationthe reaction solution was concentrated under reduced pressure
  3. custompurified by preparative HPLC

Sources & evidence

ORD record
ord-a5ee6651c89a4c23bcae8a152be3d4ef
Source dataset
uspto-grants-2013_05
Patent number
US08440666B2

Reaction notes

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