Trimethyl Phosphate → HCID 178502937, compound

HRID 1168025Notes

Reaction equation

[I-].[C:2]1([S+:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[P:21](OC)([O:25][CH3:26])([O:23][CH3:24])=[O:22]>>[CH3:24][O:23][PH:21](=[O:22])[O:25][CH3:26].[C:15]1([S+:8]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

Participants

Reactant 2

HCID 10541Trimethyl Phosphate

HCID 21881071Triphenylsulfonium iodide

Product 1

HCID 178502937HCID 178502937, compoundYield 75%

Conditions

Temperature: 130 °C

Procedure

A mixture of triphenylsulfonium iodide (390 mg; 1 mmol) and trimethyl phosphate (1 g) was stirred at 130° C. for 3 hours. Subsequently, the homogenous solution was cooled, and the thus-obtained solid matter was washed with IPA, to thereby yield 280 mg of the target compound as white crystals (yield: 72.2%). The anion content of the resultant compound was determined by ion chromatography. The iodide anion content was determined to be not greater than 50 ppm.

Workup

temperatureSubsequently, the homogenous solution was cooled
washthe thus-obtained solid matter was washed with IPA

Sources & evidence

ORD record: ord-3e2c4f206b8748ee8d145081cbc59692
Source dataset: uspto-grants-2003_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06620957B1

Reaction notes

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