Ammonia → 1-(4'-Amino-3'-trifluoromethyl-phenyl)-2-tert.pentylamino-ethanol hydrobromide

HRID 1111938ノート

反応式

HRID 1111938 の反応式
Cl.[NH2:2][C:3]1[C:8]([C:9]([F:12])([F:11])[F:10])=[CH:7][C:6]([CH:13]([OH:21])[CH2:14][NH:15][C:16]([CH2:19][CH3:20])([CH3:18])[CH3:17])=[CH:5][C:4]=1[Br:22].N.[H][H]>C(OCC)(=O)C>[BrH:22].[NH2:2][C:3]1[CH:4]=[CH:5][C:6]([CH:13]([OH:21])[CH2:14][NH:15][C:16]([CH2:19][CH3:20])([CH3:17])[CH3:18])=[CH:7][C:8]=1[C:9]([F:10])([F:11])[F:12]

参加物

5

反応物 3

HCID 222AmmoniaHCID 133556401-(4'-Amino-3'-bromo-5'-trifluoromethyl-phenyl)-2-tert.pentylamino-ethanol hydrochlorideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 133557631-(4'-Amino-3'-trifluoromethyl-phenyl)-2-tert.pentylamino-ethanol hydrobromide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

5 gm of 1-(4'-amino-3'-bromo-5'-trifluoromethyl-phenyl)-2-tert.pentylamino-ethanol hydrochloride were distributed between ethyl acetate and 2N ammonia. The organic layer was dried and evaporated in vacuo, the residual base was dissolved in 100 ml of methanol in a hydrogenation vessel. 2.5 gm of palladium oxide/barium sulfate catalyst (5%) were added, and the mixture was hydrogenated until 1 mol of hydrogen had been absorbed. After the catalyst had been removed by filtration, the filtrate was evaporated in vacuo, and the solid residue was recrystallized from isopropanol. The obtained hydrobromide melted at 174°-175° C. (decomp.).

後処理

  1. customThe organic layer was dried
  2. customevaporated in vacuo
  3. dissolutionthe residual base was dissolved in 100 ml of methanol in a hydrogenation vessel
  4. addition2.5 gm of palladium oxide/barium sulfate catalyst (5%) were added
  5. customhad been absorbed
  6. customAfter the catalyst had been removed by filtration
  7. customthe filtrate was evaporated in vacuo
  8. customthe solid residue was recrystallized from isopropanol

出典と根拠

ORDレコード
ord-630efa2be383451c87d948a961490177
出典データセット
uspto-grants-1978_10
特許番号
US04119710

反応ノート

読み込み中…