1545252-75-2 → HCID 19968899, compound

HRID 976145Notes

Reaction equation

HRID 976145 reaction equation
[F-:1].[F-].[F-].C(N(S([O-])([O-])=O)CC)C.[Cl:13][C:14]1[C:15]2[CH2:22][CH2:21][CH:20](O)[C:16]=2[N:17]=[CH:18][N:19]=1>C(Cl)(Cl)Cl>[Cl:13][C:14]1[C:15]2[CH2:22][CH2:21][CH:20]([F:1])[C:16]=2[N:17]=[CH:18][N:19]=1

Participants

4

Reactant 2

HCID 199689181545252-75-2HCID 178464504HCID 178464504, compound

Product 1

HCID 19968899HCID 19968899, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

Under ice cooling, 3.9 ml of diethylaminosulfite trifluoride (DAST) was added dropwise to 5.00 g of 4-chloro-7-hydroxy-5,6-dihydro-7H-cyclopenta[d]pyrimidine obtained above dissolved in 40 ml of chloroform, and the mixture was stirred at the same temperature for 10 minutes. After the solvent was removed under reduced pressure, water was added to the mixture, and the mixture was extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and condensed. The obtained residue was applied to silica gel column chromatography to obtain 3.09 g of the title compound as a yellow oily product.

Workup

  1. customobtained
  2. customAfter the solvent was removed under reduced pressure, water
  3. additionwas added to the mixture
  4. extractionthe mixture was extracted with ethyl acetate
  5. dry with materialThe extract was dried over anhydrous sodium sulfate and condensed

Sources & evidence

ORD record
ord-e6a91c6dbe8f49fa9b56be9500bb484f
Source dataset
uspto-grants-1997_03
Patent number
US05610303

Reaction notes

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