Bromine → HCID 58431340、化合物

HRID 1617414

反応式

HRID 1617414 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 24408BromineHCID 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 it was decolorized. The mixture containing unreacted starting material, desired product, and over brominated product, was rotovapped and azeotroped once with toluene. The percent by weight of desired component was determined by NMR and the mixture used without further purification. Yield: 1.62 g (61%); LC-MS: 313.0, 315.0 (M+H)+. 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H).

後処理

  1. additionThe mixture containing unreacted

出典と根拠

ORDレコード
ord-43879bc991a245a8aa8a2f1ed1fbdc23
出典データセット
uspto-grants-2014_07
特許番号
US08765734B2

関連ノート

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