Lithium Hydroxide → HCID 117833710, compound

HRID 515924Notes

Reaction equation

[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:20]([N:22]2[C@H:31]([CH3:32])[CH2:30][C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH2:23]2)=[O:21])=[C:6]([C:8]2[N:12]([CH3:13])[C:11]([CH3:14])=[C:10]([C:15]([O:17]CC)=[O:16])[CH:9]=2)[CH:7]=1.[Li+].[OH-].[NH4+].[Cl-]>O1CCOCC1.O.ClCCl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:20]([N:22]2[C@H:31]([CH3:32])[CH2:30][C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[CH2:23]2)=[O:21])=[C:6]([C:8]2[N:12]([CH3:13])[C:11]([CH3:14])=[C:10]([C:15]([OH:17])=[O:16])[CH:9]=2)[CH:7]=1

Participants

Conditions

Temperature: 100 °C

Procedure

To a solution of 1.7 g of the compound obtained in Step A (3.77 mmol) in 5 mL of dioxane there is added 0.317 g of LiOH (7.5 mmol) dissolved in 5 mL of water. The batch is heated in a microwave apparatus for 4 hours at 100° C. (power 140 W). The reaction mixture is then filtered and concentrated to dryness. The residue thereby obtained is taken up in dichloromethane (50 mL) and then saturated aqueous NH4Cl solution is added thereto. The organic phase is washed with water and then with brine, dried over MgSO4, filtered and concentrated to dryness. The title product is obtained in the form of a solid and is used directly in the next Step.

Workup

filtrationThe reaction mixture is then filtered
concentrationconcentrated to dryness
customThe residue thereby obtained
washThe organic phase is washed with water
dry with materialwith brine, dried over MgSO4
filtrationfiltered
concentrationconcentrated to dryness

Sources & evidence

ORD record: ord-9b3854d35b784782b5dff68d80ad646b
Source dataset: uspto-grants-2015_08
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09108983B2

Reaction notes

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