Lithium Hydroxide → HCID 57807502, compound

HRID 2267275Notes

Reaction equation

HRID 2267275 reaction equation
[Li+].[OH-].[NH2:3][C:4]1[C:9]([C:10]([F:13])([F:12])[F:11])=[CH:8][C:7]([CH2:14][C@@H:15]([O:36][C:37]([N:39]2[CH2:44][CH2:43][CH:42]([N:45]3[CH2:51][CH2:50][C:49]4[CH:52]=[CH:53][CH:54]=[CH:55][C:48]=4[NH:47][C:46]3=[O:56])[CH2:41][CH2:40]2)=[O:38])[C:16]([N:18]2[CH2:23][CH2:22][CH:21]([N:24]3[CH2:29][CH2:28][C:27]([CH3:35])([C:30]([O:32]CC)=[O:31])[CH2:26][CH2:25]3)[CH2:20][CH2:19]2)=[O:17])=[CH:6][C:5]=1[Cl:57]>O.C1COCC1>[NH2:3][C:4]1[C:9]([C:10]([F:12])([F:11])[F:13])=[CH:8][C:7]([CH2:14][C@@H:15]([O:36][C:37]([N:39]2[CH2:40][CH2:41][CH:42]([N:45]3[CH2:51][CH2:50][C:49]4[CH:52]=[CH:53][CH:54]=[CH:55][C:48]=4[NH:47][C:46]3=[O:56])[CH2:43][CH2:44]2)=[O:38])[C:16]([N:18]2[CH2:19][CH2:20][CH:21]([N:24]3[CH2:29][CH2:28][C:27]([CH3:35])([C:30]([OH:32])=[O:31])[CH2:26][CH2:25]3)[CH2:22][CH2:23]2)=[O:17])=[CH:6][C:5]=1[Cl:57]

Participants

5

Reactant 2

HCID 3939Lithium HydroxideHCID 57807424HCID 57807424, compound

Product 1

HCID 57807502HCID 57807502, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Conditions

Temperature
50 °C

Procedure

A solution of 2.00 mg (0.08 mmol) LiOH in 1 mL water was added to 40 mg (0.05 m mol) ethyl 1′-{(R)-3-(4-amino-3-chloro-5-trifluoromethyl -phenyl)-2-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carbonyloxy]-propionyl}-4-methyl-1,4′-bipiperidinyl-4-carboxylate in 0.8 mL THF and the reaction mixture was stirred for 1 h at RT and for 8 h at 50° C. This was purified by HPLC without working up; the fractions containing the product were combined and lyophilised.

Workup

  1. customThis was purified by HPLC
  2. additionthe fractions containing the product

Sources & evidence

ORD record
ord-787ab99955b343f78ff7ed4c8640c6a1
Source dataset
uspto-grants-2010_12
Patent number
US07858622B2

Reaction notes

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