Triethylsilane → 3-Methyl-6-(2-bromoethyl)benzothiazolinone

HRID 487550노트

반응식

HRID 487550 반응식
[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](=[O:15])[CH2:3]1.C([SiH](CC)CC)C>FC(F)(F)C(O)=O>[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](=[O:15])[CH2:3]1

참가 물질

4

반응물 2

HCID 12052TriethylsilaneHCID 867466573-Methyl-6-(bromoacetyl)benzothiazolinone

생성물 1

HCID 701838363-Methyl-6-(2-bromoethyl)benzothiazolinone

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

In a 500-cm3 ground-necked flask surmounted by a condenser and placed in an oil bath, 42.9 g (0.15 mol) of 3-methyl-6-(bromoacetyl)benzothiazolinone are dissolved in 77 cm3 of trifluoroacetic acid with magnetic stirring and while the temperature is stabilized at 60° C. 52.7 cm3 (0.33 mol) of triethylsilane are introduced dropwise via a dropping funnel. After the addition, the heating is stopped and the mixture is left stirring vigorously for 30 hours. The reaction medium is hydrolyzed by pouring it into ice-cold water, and the precipitate obtained is drained and washed with water until the filtrate is neutral and then with hexane. The product is dried and recrystallized in cyclohexane.

후처리

  1. customIn a 500-cm3 ground-necked flask surmounted by a condenser
  2. customplaced in an oil bath
  3. customis stabilized at 60° C
  4. additionAfter the addition
  5. waitthe mixture is left
  6. stirringstirring vigorously for 30 hours
  7. additionby pouring it into ice-cold water
  8. customthe precipitate obtained
  9. washwashed with water until the filtrate
  10. customThe product is dried
  11. customrecrystallized in cyclohexane

출처 및 근거

ORD 기록
ord-b86df02b622a45e99c31a7d627b06611
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05296477

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