Hydrochloric Acid → HCID 59676836, compound

HRID 2104454Notes

Reaction equation

HRID 2104454 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([C:11]([NH:13][C@H:14]1[C@H:18]([NH:19][C:20]([C:22]3[S:23][C:24]4[CH2:25][N:26]([CH3:31])[CH2:27][CH2:28][C:29]=4[N:30]=3)=[O:21])[CH2:17][N:16]([S:32]([CH2:35][C:36]([O:38]C)=[O:37])(=[O:34])=[O:33])[CH2:15]1)=[O:12])=[CH:5]2.O.[OH-].[Li+].Cl>O1CCCC1.O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[NH:7][C:6]([C:11]([NH:13][C@H:14]1[C@H:18]([NH:19][C:20]([C:22]3[S:23][C:24]4[CH2:25][N:26]([CH3:31])[CH2:27][CH2:28][C:29]=4[N:30]=3)=[O:21])[CH2:17][N:16]([S:32]([CH2:35][C:36]([OH:38])=[O:37])(=[O:34])=[O:33])[CH2:15]1)=[O:12])=[CH:5]2

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 59676768HCID 59676768, compound

Product 1

HCID 59676836HCID 59676836, compoundYield 89.1%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent

Procedure

The compound (100 mg) obtained in Example 100 was dissolved in tetrahydrofuran (4 mL)-water (1 mL), and the mixture was cooled with ice. Lithium hydroxide monohydrate (7.8 mg) was added thereto. The temperature of the resultant mixture was returned to room temperature, and the mixture was stirred for 4 hours. After the reaction mixture was neutralized with 1N hydrochloric acid, it was concentrated. Precipitates were collected by filtration, washed with water and 50% ethanol and dried overnight at 50° C. under reduced pressure to give the title compound (87 mg).

Workup

  1. temperaturethe mixture was cooled with ice
  2. customwas returned to room temperature
  3. concentrationwas concentrated
  4. customPrecipitates
  5. filtrationwere collected by filtration
  6. washwashed with water and 50% ethanol
  7. customdried overnight at 50° C. under reduced pressure

Sources & evidence

ORD record
ord-98090df9986d48ceb5e3b89574bccbc0
Source dataset
uspto-grants-2009_08
Patent number
US07576135B2

Reaction notes

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