Lithium Hydroxide → HCID 86632303, compound

HRID 643600Notes

Reaction equation

HRID 643600 reaction equation
[Li+].[OH-:2].[O:3]=[C:4]1[N:10]([CH:11]2[CH2:16][CH2:15][N:14]([C:17]([O:19][C@@H:20](OC)[C:21](=C=O)[C:22]3[CH:27]=[C:26]([C:28]([F:31])([F:30])[F:29])[CH:25]=[C:24]([C:32]([F:35])([F:34])[F:33])[CH:23]=3)=[O:18])[CH2:13][CH2:12]2)[CH2:9][CH2:8][C:7]2[CH:40]=[CH:41][CH:42]=[CH:43][C:6]=2[NH:5]1.C1[CH2:48][O:47]CC1>O>[O:3]=[C:4]1[N:10]([CH:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C@@H:20]([C:48]([OH:47])=[O:2])[CH2:21][C:22]3[CH:27]=[C:26]([C:28]([F:30])([F:31])[F:29])[CH:25]=[C:24]([C:32]([F:35])([F:33])[F:34])[CH:23]=3)=[O:18])[CH2:15][CH2:16]2)[CH2:9][CH2:8][C:7]2[CH:40]=[CH:41][CH:42]=[CH:43][C:6]=2[NH:5]1

Participants

5

Reactant 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 86632304HCID 86632304, compound

Product 1

HCID 86632303HCID 86632303, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 307 mg (12.8 mmol) LiOH in 5 mL water was added to a solution of 5.0 g (8.5 mmol) of (R)-2-(3,5-bis-trifluoromethyl-phenyl)-1-methoxy-carbonyl-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 50 mL THF and the reaction mixture was stirred overnight at RT. The mixture was evaporated down in vacuo, the residue was taken up in water, acidified with 1 M HCl, the precipitate was filtered off and dried in the vacuum drying cupboard at 40° C.

Workup

  1. customThe mixture was evaporated down in vacuo
  2. filtrationthe precipitate was filtered off
  3. customdried in the vacuum
  4. customdrying cupboard at 40° C.

Sources & evidence

ORD record
ord-fe73d04103f9469591b16989dc300a46
Source dataset
uspto-grants-2010_04
Patent number
US07700598B2

Reaction notes

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