HCID 14855594、化合物 → HCID 14855595、化合物

HRID 477411ノート

反応式

HRID 477411 の反応式
[F:1][C:2]1[CH:14]=[C:13]([O:15][C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-])=O)=[CH:18][C:17]=2[F:25])[CH:12]=[CH:11][C:3]=1[O:4][CH:5]([CH3:10])[C:6]([O:8][CH3:9])=[O:7]>C(O)C.[Pd]>[NH2:22][C:19]1[CH:20]=[CH:21][C:16]([O:15][C:13]2[CH:12]=[CH:11][C:3]([O:4][CH:5]([CH3:10])[C:6]([O:8][CH3:9])=[O:7])=[C:2]([F:1])[CH:14]=2)=[C:17]([F:25])[CH:18]=1

参加物

4

反応物 1

HCID 14855594HCID 14855594、化合物

生成物 1

HCID 14855595HCID 14855595、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A mixture of methyl 2-(2-fluoro-4-(2-fluoro-4-nitrophenoxy)phenoxy)propanoate (6.5 g, 0.018 mole) in ethanol (150 ml) containing 5 percent palladium on charcoal (0.5 g) as catalyst was subjected to hydrogenation (initial pressure equals 50 psi) on a Parr apparatus. After 19 hours, the excess hydrogen was removed and nitrogen was bubbled through the liquid mixture. This mixture was filtered through celite and the ethanol removed by distillation. A slightly yellow oil weighting 5.8 grams (98 percent) resulted. NMR spectroscopy (1H, 19F) and infrared (I.R.) spectroscopy confirmed the structure as one being consistent with the desired product. It was used directly in the next step without further purification.

後処理

  1. customthe excess hydrogen was removed
  2. customnitrogen was bubbled through the liquid mixture
  3. filtrationThis mixture was filtered through celite
  4. customthe ethanol removed by distillation
  5. customA slightly yellow oil weighting 5.8 grams (98 percent) resulted

出典と根拠

ORDレコード
ord-4e1965e0d3a84b6fbce03b91ef6d9981
出典データセット
uspto-grants-1989_12
特許番号
US04888050

反応ノート

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