Methane → HCID 66733858、化合物

HRID 1929616ノート

反応式

HRID 1929616 の反応式
[CH2:1]([O:5][C:6](=[O:18])[CH:7]=[CH:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4].C>[Pd].CO>[CH2:1]([O:5][C:6](=[O:18])[CH2:7][CH2:8][C:9]1[CH:14]=[C:13]([F:15])[C:12]([CH3:16])=[C:11]([F:17])[CH:10]=1)[CH2:2][CH2:3][CH3:4]

参加物

5

反応物 2

HCID 297MethaneHCID 66733998HCID 66733998、化合物

生成物 1

HCID 66733858HCID 66733858、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of 3-(3,5-difluoro-4-methyl-phenyl)-acrylic acid butyl ester (7.651 g; 30.089 mmol) and 10% palladium over activated charcoal (0.760 g) was placed under nitrogen before MeOH (100 ml) was carefully added. The resulting suspension was placed under vacuum, then under hydrogen (1 atm), and the reaction mixture was vigorously stirred at rt for 2 h45. The reaction mixture was filtered over a pad of celite, and concentrated under reduced pressure to give the expected product 3-(3,5-difluoro-4-methyl-phenyl)-propionic acid butyl ester as a yellow oil which was further dried under HV (6.960 g; 90%). LC-MS: tR=1.10 min; [M+H]+: no ionisation.

後処理

  1. additionwas carefully added
  2. filtrationThe reaction mixture was filtered over a pad of celite
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f22a620250634a2eb9b20ad420dd3967
出典データセット
uspto-grants-2012_05
特許番号
US08188082B2

反応ノート

読み込み中…