Lithium hydroxide, monohydrate → HCID 86623313, compound

HRID 1873499Notes

Reaction equation

HRID 1873499 reaction equation
[C:1]([O:5][C:6]([C:8]1[CH2:9][C:10]([C:26]([O:28]CC)=[O:27])=[CH:11][C:12]2[CH:18]=[CH:17][C:16]([C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21])=[CH:15][C:13]=2[N:14]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O[Li].O>C1COCC1.O>[C:1]([O:5][C:6]([C:8]1[CH2:9][C:10]([C:26]([OH:28])=[O:27])=[CH:11][C:12]2[CH:18]=[CH:17][C:16]([C:19]([F:25])([F:24])[C:20]([F:21])([F:23])[F:22])=[CH:15][C:13]=2[N:14]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

Participants

4

Reactant 2

HCID 168937Lithium hydroxide, monohydrateHCID 86623312HCID 86623312, compound

Product 1

HCID 86623313HCID 86623313, compound

Reagents, catalysts & solvents 1

HCID 21881883Oxolane--water (1/1)Solvent

Procedure

To a solution of (1E,4E)-ethyl 2-(tert-butoxycarbonyl)-8-(perfluoroethyl)-3H-benzo[b]azepine-4-carboxylate in THF/H2O (4:1, 10 mL) was added LiOH.H2O (42 mg, 1.00 mmol). After 4 hours the mixture was made acidic (pH 4) with 10% citric acid and extracted with CH2Cl2 (2×100 mL). The combined organics were dried and concentrated. The material was used without further purification.

Workup

  1. extraction(pH 4) with 10% citric acid and extracted with CH2Cl2 (2×100 mL)
  2. customThe combined organics were dried
  3. concentrationconcentrated
  4. customThe material was used without further purification

Sources & evidence

ORD record
ord-369050cf7d354424bf083b40864e167b
Source dataset
uspto-grants-2012_11
Patent number
US08304407B2

Reaction notes

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