Lithium Hydroxide → HCID 67301680, compound

HRID 641252Notes

Reaction equation

HRID 641252 reaction equation
[Li+].[OH-].[O:3]=[C:4]1[N:10]([CH:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C@@H:20]([C:30]([O:32]C)=[O:31])[CH2:21][C:22]3[CH:23]=[N:24][C:25]([NH2:29])=[C:26]([CH3:28])[CH:27]=3)=[O:18])[CH2:13][CH2:12]2)[CH2:9][CH2:8][C:7]2[CH:34]=[CH:35][CH:36]=[CH:37][C:6]=2[NH:5]1>O.C1COCC1>[O:3]=[C:4]1[N:10]([CH:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C@@H:20]([C:30]([OH:32])=[O:31])[CH2:21][C:22]3[CH:23]=[N:24][C:25]([NH2:29])=[C:26]([CH3:28])[CH:27]=3)=[O:18])[CH2:15][CH2:16]2)[CH2:9][CH2:8][C:7]2[CH:34]=[CH:35][CH:36]=[CH:37][C:6]=2[NH:5]1

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 67301411HCID 67301411, compound

Product 1

HCID 67301680HCID 67301680, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of 100 mg (4.18 mmol) LiOH in 25 mL water was added to a solution of 1.27 g (2.64 mmol) of (R)-2-(6-amino-5-methyl-pyridin-3-yl)-1-methoxycarbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 30 mL THF and the reaction solution was stirred for 1 h at RT. The mixture was evaporated down i.vac., the residue was taken up in water, 2 M KHSO4 solution were added with stirring, the supernatant solution was decanted off, the residue was dried, stirred with THF and the product was filtered.

Workup

  1. customThe mixture was evaporated down i.vac
  2. addition2 M KHSO4 solution were added
  3. stirringwith stirring
  4. customthe supernatant solution was decanted off
  5. customthe residue was dried
  6. stirringstirred with THF
  7. filtrationthe product was filtered

Sources & evidence

ORD record
ord-129724e272a34f0a8b759461dae0ab5b
Source dataset
uspto-grants-2010_04
Patent number
US07696196B2

Reaction notes

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