Lithium hydroxide, monohydrate → HCID 68609264, compound

HRID 642814Notes

Reaction equation

HRID 642814 reaction equation
O.[OH-].[Li+].C([O:6][C:7]([C@H:9]([O:28][C:29]([N:31]1[CH2:36][CH2:35][CH:34]([N:37]2[CH2:43][CH2:42][C:41]3[CH:44]=[CH:45][CH:46]=[CH:47][C:40]=3[NH:39][C:38]2=[O:48])[CH2:33][CH2:32]1)=[O:30])[CH2:10][C:11]1[CH:12]=[C:13]2[C:17](=[C:18]([CH3:20])[CH:19]=1)[N:16]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[N:15]=[CH:14]2)=[O:8])C>O.C1COCC1>[C:7]([C@H:9]([O:28][C:29]([N:31]1[CH2:32][CH2:33][CH:34]([N:37]2[CH2:43][CH2:42][C:41]3[CH:44]=[CH:45][CH:46]=[CH:47][C:40]=3[NH:39][C:38]2=[O:48])[CH2:35][CH2:36]1)=[O:30])[CH2:10][C:11]1[CH:12]=[C:13]2[C:17](=[C:18]([CH3:20])[CH:19]=1)[N:16]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[N:15]=[CH:14]2)([OH:8])=[O:6]

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 68610254HCID 68610254, compound

Product 1

HCID 68609264HCID 68609264, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

A solution of 19.2 mg (0.8 mmol) lithium hydroxide hydrate in 10 mL water was added at RT to a solution of 330 mg (0.53 mmol) tert.-butyl 5-{(R)-2-ethoxycarbonyl-2-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidine-1-carbonyloxy]-ethyl}-7-methyl-indazol-1-carboxylate in 30 mL THF and the reaction mixture was stirred for 30 min at RT. It was evaporated down i.vac., the residue was taken up in 100 mL water, combined with 10% citric acid with stirring, extracted twice with 100 mL DCM and the combined organic phases were dried over Na2SO4. After the desiccant and solvent had been eliminated the residue was reacted further without purification.

Workup

  1. customIt was evaporated down i.vac
  2. stirringwith stirring
  3. extractionextracted twice with 100 mL DCM
  4. dry with materialthe combined organic phases were dried over Na2SO4
  5. customwas reacted further without purification

Sources & evidence

ORD record
ord-161a2732b4094cfe9be4b6e2614a7b65
Source dataset
uspto-grants-2010_04
Patent number
US07696195B2

Reaction notes

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