Acetic Acid → HCID 178426049、化合物

HRID 2106799ノート

反応式

HRID 2106799 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178426049HCID 178426049、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ff2ef003c4d04db19975118f21bb61c2
出典データセット
uspto-grants-1990_06
特許番号
US04931452

反応ノート

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