Water → HCID 12884911, compound

HRID 466334Notes

Reaction equation

HRID 466334 reaction equation
[CH3:1][Ge:2]([CH3:20])([CH3:19])[C:3]1[CH:4]=[C:5]([C:13]2([CH3:18])OCC[O:14]2)[CH:6]=[C:7]([Ge:9]([CH3:12])([CH3:11])[CH3:10])[CH:8]=1.CC1C=CC(S([O-])(=O)=O)=CC=1.C1C=C[NH+]=CC=1.O>CC(C)=O>[CH3:11][Ge:9]([CH3:10])([CH3:12])[C:7]1[CH:6]=[C:5]([C:13](=[O:14])[CH3:18])[CH:4]=[C:3]([Ge:2]([CH3:19])([CH3:1])[CH3:20])[CH:8]=1

Participants

5

Reactant 3

HCID 962WaterHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 128849082-(3,5-Bis(trimethylgermyl)phenyl]-2-methyl-1,3-dioxolane

Product 1

HCID 12884911HCID 12884911, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

A mixture of 240 mg (0.60 mmol) of 2-[3,5-bis(trimethylgermyl)phenyl]-2-methyl-1,3-dioxolane, 23 mg (0.090 mmol) of PPTS, 10.6 ml of acetone (excess) and 540 mg (30 mmol) of water was refluxed for 2.5 hours. The reaction mixture was evaporated and extracted with ether. The extract was evaporated to give 208 mg of pale yellow crystals, which were sublimed at 70° C., 0.5 mmHg to give 189 mg of white prisms, m.p. 56° C. (yield 89%).

Workup

  1. temperaturewas refluxed for 2.5 hours
  2. customThe reaction mixture was evaporated
  3. extractionextracted with ether
  4. customThe extract was evaporated

Sources & evidence

ORD record
ord-84c76dfadd7e48b6a8d36e4e9f59f2ef
Source dataset
uspto-grants-1992_10
Patent number
US05155249

Reaction notes

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