Bromine → HCID 58431340、化合物

HRID 1426309

反応式

HRID 1426309 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:3]=1.[Br:17]Br>C(O)(=O)C>[Br:17][CH2:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:3]=1

参加物

4

反応物 2

HCID 24408Bromine2 回HCID 67390769Ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate

生成物 1

HCID 58431340HCID 58431340、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

A solution of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (2.00 g, 8.54 mmol, prepared as described in WO2007/090748) in acetic acid (12 mL) was treated with bromine (1.36 g, 8.54 mmol) and the reaction was heated to 80° C. in a sealed vial for 30 minutes, at which time, the color of bromine was dissipated. The acetic acid was removed in vacuo and was followed by dissolving of the residue in toluene and removal of solvent in vacuo. The percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product) was determined by NMR and the mixture used without further purification (1.62 g, 61%). 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H); LCMS (M+H)+: 313.0, 315.0

後処理

  1. customThe acetic acid was removed in vacuo
  2. dissolutionby dissolving of the residue in toluene
  3. customremoval of solvent in vacuo
  4. additionThe percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product)
  5. customthe mixture used without further purification (1.62 g, 61%)

出典と根拠

ORDレコード
ord-0a72c58090a64fdbb1ebd67d96e5bb41
出典データセット
uspto-grants-2015_01
特許番号
US08933085B2

関連ノート

読み込み中…