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1,1,1-Trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-{[(phenylmethyl)amino]methyl}-2-pentanol → 2-(Aminomethyl)-1,1,1-trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-pentanol

HRID 418777
ノート
印刷プレビュー

反応式

HRID 418777 の反応式
[F:1][C:2]([F:28])([F:27])[C:3]([CH2:18][NH:19]CC1C=CC=CC=1)([OH:17])[CH2:4][C:5]([C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])([CH3:7])[CH3:6].[H][H]>C(O)C.[Pd]>[NH2:19][CH2:18][C:3]([OH:17])([CH2:4][C:5]([C:8]1[CH:13]=[C:12]([F:14])[CH:11]=[CH:10][C:9]=1[O:15][CH3:16])([CH3:7])[CH3:6])[C:2]([F:28])([F:27])[F:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 576159391,1,1-Trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-{[(phenylmethyl)amino]methyl}-2-pentanol2 回HCID 178418361HCID 178418361、化合物

生成物 1

HCID 179365862-(Aminomethyl)-1,1,1-trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-pentanol収率 97.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol
溶媒

実験手順

1,1,1-Trifluoro-4-[5-fluoro-2-(methyloxy)phenyl]-4-methyl-2-{[(phenylmethyl)amino]methyl}-2-pentanol (Intermediate 17, 63 g, 0.158 mol) was added to a stirred solution of 10% Pd/C (12.6 g, 50% wet) in ethanol (1.07 L) at 20° C. in a nitrogen purged vessel. The mixture was hydrogenated at 20° C. and atmospheric pressure until there was no further hydrogen uptake. The suspension was then filtered through Celite and glass fibre filter paper to remove the catalyst, and the cake washed with ethanol (120 mL). The combined filtrate and washings were evaporated under reduced pressure to give the title compound as a light grey solid (47.5 g).

後処理

  1. customwas hydrogenated at 20° C.
  2. filtrationThe suspension was then filtered through Celite and glass fibre filter paper
  3. customto remove the catalyst
  4. washthe cake washed with ethanol (120 mL)
  5. customThe combined filtrate and washings were evaporated under reduced pressure

出典と根拠

ORDレコード
ord-c668de29d48740daa33fa42f76e54478
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08093281B2

反応ノート

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