Lithium Hydroxide → HCID 57807686, compound

HRID 2267266Notes

Reaction equation

HRID 2267266 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]([CH2:41][C:42]3[CH:47]=[C:46]([C:48]([F:51])([F:50])[F:49])[C:45]([NH2:52])=[C:44]([Cl:53])[CH:43]=3)[C:21]([N:23]3[CH2:28][CH2:27][CH:26]([N:29]4[CH2:34][CH2:33][CH:32](C(OCC)=O)[CH2:31][CH:30]4C)[CH2:25][CH2:24]3)=[O:22])=[O:18])[CH2:13][CH2:12]2)[CH2:9][CH2:8][C:7]2[CH:54]=[CH:55][CH:56]=[CH:57][C:6]=2[NH:5]1.[CH2:58]1[CH2:62][O:61]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]([CH2:41][C:42]3[CH:47]=[C:46]([C:48]([F:51])([F:49])[F:50])[C:45]([NH2:52])=[C:44]([Cl:53])[CH:43]=3)[C:21]([N:23]3[CH2:24][CH2:25][CH:26]([N:29]4[CH2:34][CH2:33][CH:32]([CH2:58][C:62]([OH:2])=[O:61])[CH2:31][CH2:30]4)[CH2:27][CH2:28]3)=[O:22])=[O:18])[CH2:15][CH2:16]2)[CH2:9][CH2:8][C:7]2[CH:54]=[CH:55][CH:56]=[CH:57][C:6]=2[NH:5]1

Participants

5

Reactant 3

HCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 131727598HCID 131727598, compound

Product 1

HCID 57807686HCID 57807686, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A solution of 5.00 mg (0.21 mmol) LiOH in 3 mL water was added to 100 mg (0.13 mmol) (R)-1-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-2-(4-ethoxycarbonyl-methyl-1,4′-bipiperidinyl-1′-yl)-2-oxo-ethyl 4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carboxylate in 10 mL THF and the reaction mixture was stirred for 2 days at RT. The mixture was evaporated to dryness i. vac., the residue was taken up in 1 mL DMF and purified by HPLC; the fractions containing the product were combined and lyophilised.

Workup

  1. customThe mixture was evaporated to dryness i
  2. custompurified by HPLC
  3. additionthe fractions containing the product

Sources & evidence

ORD record
ord-a2ab7edb7cad4368b7879083de68aaeb
Source dataset
uspto-grants-2010_12
Patent number
US07858622B2

Reaction notes

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