Lithium hydroxide, monohydrate → HCID 59899152, compound

HRID 2227286Notes

Reaction equation

HRID 2227286 reaction equation
C([O:3][C:4](=[O:36])[CH2:5][C@@H:6]([C:29]1[CH:30]=[N:31][C:32]([CH3:35])=[N:33][CH:34]=1)[CH2:7][CH2:8][CH2:9][N:10]1[C@H:14]([CH3:15])[CH2:13][C@H:12]([NH:16][CH2:17][C:18]2[CH:27]=[CH:26][C:25]3[CH2:24][CH2:23][CH2:22][NH:21][C:20]=3[N:19]=2)[C:11]1=[O:28])C.O.[OH-].[Li+]>O1CCCC1.O>[CH3:35][C:32]1[N:33]=[CH:34][C:29]([C@@H:6]([CH2:7][CH2:8][CH2:9][N:10]2[C@H:14]([CH3:15])[CH2:13][C@H:12]([NH:16][CH2:17][C:18]3[CH:27]=[CH:26][C:25]4[CH2:24][CH2:23][CH2:22][NH:21][C:20]=4[N:19]=3)[C:11]2=[O:28])[CH2:5][C:4]([OH:36])=[O:3])=[CH:30][N:31]=1

Participants

5

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 59899161HCID 59899161, compound

Product 1

HCID 59899152HCID 59899152, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

To a stirred solution of 5-6 (110 mg) in tetrahydrofuran (4.5 mL) was added lithium hydroxide monohydrate (45 mg) in water (4.5 mL) and the mixture was stirred for 16 h. The reaction mixture was concentrated at reduced pressure and the resulting oil was purified by flash column chromatography (silica gel, 30:3:3 to 50:5:5% ethanol/ammonium hydroxide/water in ethyl acetate) to give 5-7 as a white solid.

Workup

  1. concentrationThe reaction mixture was concentrated at reduced pressure
  2. customthe resulting oil was purified by flash column chromatography (silica gel, 30:3:3 to 50:5:5% ethanol/ammonium hydroxide/water in ethyl acetate)

Sources & evidence

ORD record
ord-dd78ab143d104011b6874d2cd1a9c98c
Source dataset
uspto-grants-2002_07
Patent number
US06413955B1

Reaction notes

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