(Diethylamino)sulfur trifluoride → HCID 18662971, compound

HRID 1956174Notes

Reaction equation

HRID 1956174 reaction equation
O[C:2]1([C:18]2[C:19]([O:24][CH3:25])=[N:20][CH:21]=[N:22][CH:23]=2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[O:7][CH2:6][O:5][C:4]2[CH:14]=[CH:15][CH:16]=[CH:17][C:3]1=2.C(N(S(F)(F)[F:32])CC)C>ClCCl>[F:32][C:2]1([C:18]2[C:19]([O:24][CH3:25])=[N:20][CH:21]=[N:22][CH:23]=2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=2[O:7][CH2:6][O:5][C:4]2[CH:14]=[CH:15][CH:16]=[CH:17][C:3]1=2

Participants

4

Reactant 2

HCID 123472(Diethylamino)sulfur trifluorideHCID 18662972HCID 18662972, compound

Product 1

HCID 18662971HCID 18662971, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture of 0.8 g of 5-(12-hydroxydibenzo[d,g][1,3]dioxocin-12-yl)-4-methoxypyrimidine, 1 mL of DAST (diethylaminosulfur trifluoride) and 30 mL of dichloromethane was prepared and allowed to stir at ambient temperature overnight. The mixture was then washed with water, dried over sodium sulfate, and concentrated by evaporation under reduced pressure. The residue was recrystallized from a mixture of dichloromethane and hexane to obtain 0.25 g of the title compound as a white solid.

Workup

  1. customwas prepared
  2. washThe mixture was then washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated by evaporation under reduced pressure
  5. customThe residue was recrystallized from a mixture of dichloromethane and hexane

Sources & evidence

ORD record
ord-05fd653f471241cfae3196cd9fbdff7b
Source dataset
uspto-grants-1998_07
Patent number
US05780465

Reaction notes

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