Acetic Acid → HCID 178426049, 화합물

HRID 2106799노트

반응식

HRID 2106799 반응식
Br.C[O:3][C:4]1[C:9]([CH3:10])=[CH:8][C:7]([C:11]([F:14])([F:13])[F:12])=[CH:6][N:5]=1.C(O)(=O)C>O>[CH3:10][C:9]1[C:4]([OH:3])=[N:5][CH:6]=[C:7]([C:11]([F:14])([F:12])[F:13])[CH:8]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 111168552-Methoxy-3-methyl-5-(trifluoromethyl)pyridine

생성물 1

HCID 178426049HCID 178426049, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Two ml of 48 percent hydrobromic acid were added with stirring to mixture of 1.38 g (5.5 mol) of 2-methoxy-3-methyl-5-(trifluoromethyl)pyridine and 6 ml of glacial acetic acid at 100° C. and the mixture was allowed to react at about 95° C. for 20 min. The mixture was then cooled and poured onto ice and the solid that formed was collected by filtration. A second crop of solid was obtained by adding more water to the filtrate. The combined solids were dried to obtain 0.40 g (40 percent of theory) of the title compound as a white powder melting at 141°-143° C. The proton nmr spectrum was consistent with the assigned structure.

후처리

  1. customto react at about 95° C. for 20 min
  2. temperatureThe mixture was then cooled
  3. additionpoured onto ice
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. customA second crop of solid was obtained
  7. customThe combined solids were dried

출처 및 근거

ORD 기록
ord-ff2ef003c4d04db19975118f21bb61c2
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04931452

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