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4-Methyl-3-nitro-1,1,1-trifluoro-2-pentanol → 3-Amino-1,1,1-trifluoro-4-methylpentan-2-ol

HRID 1598891
ノート
印刷プレビュー

反応式

HRID 1598891 の反応式
[CH3:1][CH:2]([CH3:13])[CH:3]([N+:10]([O-])=O)[CH:4]([OH:9])[C:5]([F:8])([F:7])[F:6].[H][H]>C(O)(C)C.C(O)(=O)C.[Pd]>[NH2:10][CH:3]([CH:2]([CH3:13])[CH3:1])[CH:4]([OH:9])[C:5]([F:6])([F:7])[F:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 187920764-Methyl-3-nitro-1,1,1-trifluoro-2-pentanolHCID 178418361HCID 178418361、化合物

生成物 1

HCID 145032463-Amino-1,1,1-trifluoro-4-methylpentan-2-ol

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 3776Isopropanol溶媒

反応条件

温度
5 °C

実験手順

A solution of 4-methyl-3-nitro-1,1,1-trifluoro-2-pentanol (17.1 g) in isopropanol (115 ml) and acetic acid (0.43 ml) was hydrogenated over 10% palladium on carbon (2.4 g) at 3.5 barg pressure until uptake of hydrogen was complete. The catalyst was removed by filtration through diatomaceous earth and the filter cake washed with isopropanol. The filtrate was evaporated under vacuum until no further isopropanol distilled and the residue dissolved in acetonitrile (40 ml). A solution of oxalic acid (3.94 g) in acetonitrile (80 ml) was added with stirring and the mixture cooled to 5° C. The product which crystallised was collected by filtration, washed with cold acetonitrile and dried at 50° C. to give 3-amino-4-methyl-1,1,1-trifluoro-2-pentanol as its oxalate salt (9.08 g). ##STR4##

後処理

  1. customThe catalyst was removed by filtration through diatomaceous earth
  2. washthe filter cake washed with isopropanol
  3. customThe filtrate was evaporated under vacuum until no further isopropanol
  4. distillationdistilled
  5. dissolutionthe residue dissolved in acetonitrile (40 ml)
  6. additionA solution of oxalic acid (3.94 g) in acetonitrile (80 ml) was added
  7. customThe product which crystallised
  8. filtrationwas collected by filtration
  9. washwashed with cold acetonitrile
  10. customdried at 50° C.

出典と根拠

ORDレコード
ord-c3c6fac50486476e8ce6d0b7c8cde0a6
出典データセット
uspto-grants-1998_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05739157

反応ノート

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