Hydrochloric Acid → HCID 59676836, compound

HRID 902900Notes

Reaction equation

HRID 902900 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, and the resultant mixture was heated to room temperature and stirred for 4 hours. After the reaction mixture was neutralized with 1N hydrochloric acid, it was concentrated. Deposits were collected by filtration, washed with water and 50% ethanol and dried overnight at 50° C. under reduced pressure to obtain the title compound (87 mg).

Workup

  1. temperaturethe mixture was cooled with ice
  2. concentrationwas concentrated
  3. filtrationDeposits were collected by filtration
  4. washwashed with water and 50% ethanol
  5. customdried overnight at 50° C. under reduced pressure

Sources & evidence

ORD record
ord-9967d0166f644fdbad91b3148ec1e73f
Source dataset
uspto-grants-2008_04
Patent number
US07365205B2

Reaction notes

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