Trifluoroacetic acid → HCID 14995349, compound

HRID 273689Notes

Reaction equation

HRID 273689 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 tool of 3-methyl-6-bromoacetylbenzothiazolin-2-one (42.9 g) is dissolved in 1 mol of trifluoroacetic acid (77 cm3) in a 250 cm3 groundneck 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-bf0953792a874d69b4fb0298a94cebc0
Source dataset
uspto-grants-1995_02
Patent number
US05387586

Reaction notes

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