Trifluoroacetic acid → HCID 14995349, compound

HRID 1734515Notes

Reaction equation

HRID 1734515 reaction equation
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11](=O)[CH2:12][Br:13])=[CH:10][C:5]=2[S:4][C:3]1=[O:15].FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][CH2:12][Br:13])=[CH:10][C:5]=2[S:4][C:3]1=[O:15]

Participants

4

Procedure

0.15 mol of 3-methyl-6-bromoacetylbenzothiazolin-2-one (42.9 g) is dissolved in 1 mol of trifluoroacetic acid (77 cm3) in a 250 cm3 ground-neck flask. 0.33 mol of triethylsilane (52.70 cm3) is introduced dropwise using a dropping funnel, with magnetic stirring. A calcium chloride drying tube is fitted and stirring is maintained for the required time at room temperature. The reaction mixture is poured into 500 cm3 of ice-cold water. The precipitate obtained is filtered off, washed with water until the wash liquors are neutral, dried and then recrystallized.

Workup

  1. customA calcium chloride drying tube is fitted
  2. customThe precipitate obtained
  3. filtrationis filtered off
  4. washwashed with water until the wash liquors
  5. customdried
  6. customrecrystallized

Sources & evidence

ORD record
ord-722111075f1b426bbfe14f8095a72bf6
Source dataset
uspto-grants-1996_07
Patent number
US05534517

Reaction notes

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