Hydroxide → HCID 25127534, compound

HRID 1672768Notes

Reaction equation

HRID 1672768 reaction equation
Cl.Cl.[CH2:3]([NH:5][C:6]1[N:7]=[CH:8][C:9]2[C:18](=[O:19])[N:17]([CH2:20][CH:21]3[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)[CH2:16][C@H:15]3[N:11]([CH2:12][CH2:13][CH2:14]3)[C:10]=2[N:27]=1)[CH3:4].[OH-]>CO>[CH2:3]([NH:5][C:6]1[N:7]=[CH:8][C:9]2[C:18](=[O:19])[N:17]([CH2:20][CH:21]3[CH2:22][CH2:23][NH:24][CH2:25][CH2:26]3)[CH2:16][C@H:15]3[N:11]([CH2:12][CH2:13][CH2:14]3)[C:10]=2[N:27]=1)[CH3:4]

Participants

4

Reactant 2

HCID 961HydroxideHCID 67352345HCID 67352345, compound

Product 1

HCID 25127534HCID 25127534, compoundYield 102.5%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Compound 24 (1.05 g, 2.52 mmol) obtained in Example 24 was dissolved in methanol (10 mL), and the mixture was stirred at room temperature for 1 hour after adding BIO RAD AG 1-X8 Resin (BIO RAD; AG 1-X8 resin, 20-50 mesh, hydroxide form). The reaction mixture was filtrated, and the filtrate was concentrated under reduced pressure to give (S)-9-ethylamino-5-(piperidin-4-yl)methyl-1,2,3,3a,4,5-hexahydro-5,8,10,10b-tetraazabenzo[e]azulen-6-one (890 mg, quantitative).

Workup

  1. filtrationThe reaction mixture was filtrated
  2. concentrationthe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-a03bbb2af2da42dd8987b9bc5ea1b37c
Source dataset
uspto-grants-2011_08
Patent number
US07998954B2

Reaction notes

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