3-Bromo-4-(trifluoromethoxy)benzoic acid → HCID 67211313、化合物

HRID 2040532ノート

反応式

HRID 2040532 の反応式
Br[C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][C:12]([F:15])([F:14])[F:13])[C:5]([OH:7])=[O:6].[C:16]([Cu])#[N:17]>CN1CCCC1=O.ClCCl>[C:16]([C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][C:12]([F:15])([F:14])[F:13])[C:5]([OH:7])=[O:6])#[N:17]

参加物

5

反応物 2

HCID 202740913-Bromo-4-(trifluoromethoxy)benzoic acidHCID 178418546HCID 178418546、化合物

生成物 1

HCID 67211313HCID 67211313、化合物収率 86.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
200 °C

実験手順

3-Bromo-4-(trifluoromethoxy)benzoic acid (1.4 g, 4.91 mmol) and cyanocopper (0.572 g, 6.39 mmol) were mixed in N-methyl-2-pyrrolidinone (NMP) (14 mL). The mixture was heated in a microwave at 200° C. for 2 h. The reaction was diluted with dichloromethane (150 mL). Celite® was added and the mixture was stirred vigorously for 10 min. The solids were removed by filtration. The organic layer was washed with water (125 mL) and concentrated. The residue was purified by HPLC to give the title compound as an off-white solid (0.979 g). LCMS m/z=232.3 [M+H]+.

後処理

  1. additionCelite® was added
  2. customThe solids were removed by filtration
  3. washThe organic layer was washed with water (125 mL)
  4. concentrationconcentrated
  5. customThe residue was purified by HPLC

出典と根拠

ORDレコード
ord-38dcfd3944dd4869a462efdb01082ce5
出典データセット
uspto-grants-2013_11
特許番号
US08580841B2

反応ノート

読み込み中…