1-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide → HCID 68360001、化合物

HRID 518796

反応式

HRID 518796 の反応式
[I-].[CH3:2][N+:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)=[CH:5][CH:4]=1.[H][H]>CO.O.[Pt]=O>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([O:18][CH:19]([CH3:21])[CH3:20])[CH:10]=2)[CH2:5][CH2:4]1

参加物

5

反応物 2

HCID 866979641-Methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 68360001HCID 68360001、化合物収率 96.7%

試薬・触媒・溶媒 2

HCID 86587499Platinum oxide monohydrate触媒HCID 887Methanol溶媒

実験手順

A solution of 10 g of 1-methyl-4-[4-nitro-3-(propan-2-yloxy)phenyl]pyridinium iodide in 280 ml of methanol is hydrogenated in an autoclave on 2.9 g of platinum oxide hydrate, at a hydrogen pressure of 15 bar and at ambient temperature for 4 h. The catalyst is removed by filtration on Clarcel and the mixture is concentrated under vacuum. The residue is taken up in 200 ml of ethyl acetate and washed with 200 ml of 1M sodium hydroxide and then with a saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated under vacuum, so as to obtain 6.0 g of 4-(1-methylpiperidin-4-yl)-2-(propan-2-yloxy)aniline.

後処理

  1. customThe catalyst is removed by filtration on Clarcel
  2. concentrationthe mixture is concentrated under vacuum
  3. washwashed with 200 ml of 1M sodium hydroxide
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-946ca97885874ef1b5b284a4e52a64f0
出典データセット
uspto-grants-2015_08
特許番号
US09115140B2

関連ノート

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