HCID 67119435、化合物 → HCID 67119420、化合物

HRID 384833ノート

反応式

HRID 384833 の反応式
[CH3:1][C:2]1[C:13]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:25])([F:24])[F:23])=[CH:17][CH:16]=2)=[CH:12][C:5]([C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[O:7])=[C:4]([N+:26]([O-])=O)[CH:3]=1>[C].[Pd].CO>[NH2:26][C:4]1[CH:3]=[C:2]([CH3:1])[C:13]([O:14][C:15]2[CH:20]=[CH:19][C:18]([O:21][C:22]([F:23])([F:24])[F:25])=[CH:17][CH:16]=2)=[CH:12][C:5]=1[C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[O:7]

参加物

4

反応物 1

HCID 67119435HCID 67119435、化合物

生成物 1

HCID 67119420HCID 67119420、化合物収率 95.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

An 80% methanol (225 g), 50 g of isopropyl 4-methyl-2-nitro-5-(4-(trifluoromethoxy)phenoxy)benzoate, and 2.5 g of a 5% palladium carbon were charged into a 500-ml stainless steel autoclave equipped with a stirring device and a thermometer, and a reaction was allowed to proceed under a hydrogen pressure of 0.5 MPa at 30° C. for 6 hr. After the replacement of the air in the autoclave with nitrogen, the reaction solution was filtered using 220 ml of methanol to remove the catalyst. The methanol solution thus obtained was concentrated under the reduced pressure, and 208 ml of water was added to the residue. The precipitated solid was collected by filtration and was dried to give isopropyl 2-amino-4-methyl-5-(4-(trifluoromethoxy)phenoxy)benzoate (43.96 g, yield: 95%).

後処理

  1. customequipped with a stirring device
  2. customat 30° C.
  3. customfor 6 hr
  4. filtrationAfter the replacement of the air in the autoclave with nitrogen, the reaction solution was filtered
  5. customto remove the catalyst
  6. customThe methanol solution thus obtained
  7. concentrationwas concentrated under the reduced pressure, and 208 ml of water
  8. additionwas added to the residue
  9. filtrationThe precipitated solid was collected by filtration
  10. customwas dried

出典と根拠

ORDレコード
ord-49bf7e32d61f4c0bbe843588ff6d2726
出典データセット
uspto-grants-2013_02
特許番号
US08367833B2

反応ノート

読み込み中…