Dichloromethane → HCID 102262609, compound

HRID 1168660Notes

Reaction equation

HRID 1168660 reaction equation
C(Cl)Cl.CCCCCCCCCCCCCCC[C:19]1[C:24](=[O:25])[N:23]([CH3:26])[C:21](=[O:22])[C:20]=1[C:27]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[N:29]([CH3:36])[CH:28]=1.[C:37](Cl)(=[O:44])C1C=CC=CC=1.[OH-].[Na+]>O>[CH3:36][N:29]1[C:30]2[C:35](=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:27]([C:20]2[C:21](=[O:22])[N:23]([CH3:26])[C:24](=[O:25])[C:19]=2[O:44][CH3:37])=[CH:28]1

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 7412Benzoyl chlorideHCID 14798Sodium HydroxideHCID 102262611HCID 102262611, compound

Product 1

HCID 102262609HCID 102262609, compoundYield 15.5%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Into a methylene chloride (500 ml)/a triethylamine (11 g, 1.1 mol) was dissolved IM-7 (124.6 g, 1 mol). Benzoyl chloride (140.6 g, 1 mol) was added dropwise at room temperature. After the mixture was stirred for four hours, water (100 ml) and an aqueous 5% NaOH solution (50 ml) were added, then, the mixture was separated. After a methylene chloride layer was dried with magnesium sulfate, it was concentrated, then, distillated under a reduced pressure (150 to 160° C., 6 mmHg) to obtain 42 g of IM-8.

Workup

  1. customthe mixture was separated
  2. dry with materialAfter a methylene chloride layer was dried with magnesium sulfate, it
  3. concentrationwas concentrated
  4. customdistillated under a reduced pressure (150 to 160° C., 6 mmHg)

Sources & evidence

ORD record
ord-314dfafbb59147f7bd85ca76bee44d2c
Source dataset
uspto-grants-2003_09
Patent number
US06627099B2

Reaction notes

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