1-Benzyl-4-[N-ethyl-N-(6-chloro-5-nitro-4-pyrimidinyl)amino]piperidine → 1-Benzyl-4-[N-ethyl-N-(5-amino-4-pyrimidinyl)amino]piperidine

HRID 361865ノート

反応式

HRID 361865 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:25][CH3:26])[C:15]2[C:20]([N+:21]([O-])=O)=[C:19](Cl)[N:18]=[CH:17][N:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>C(O)C.[OH-].[Pd+2].[OH-]>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH2:25][CH3:26])[C:15]2[C:20]([NH2:21])=[CH:19][N:18]=[CH:17][N:16]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 544731551-Benzyl-4-[N-ethyl-N-(6-chloro-5-nitro-4-pyrimidinyl)amino]piperidine

生成物 1

HCID 542746941-Benzyl-4-[N-ethyl-N-(5-amino-4-pyrimidinyl)amino]piperidine

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

1-Benzyl-4-[N-ethyl-N-(6-chloro-5-nitro-4-pyrimidinyl)amino]piperidine (EXAMPLE 252, 3.00 g) is dissolved in 150 ml of ethanol and 0.75 g of palladium hydroxide is added. The reaction is placed on a Parr hydrogenator at 10 psi for 1 h, then filtered through diatemous earth and concentrated under reduced pressure. Purification by flash column chromatography (5% methanol/chloroform) gives the title compound.

後処理

  1. filtrationfiltered through diatemous earth
  2. concentrationconcentrated under reduced pressure
  3. customPurification by flash column chromatography (5% methanol/chloroform)

出典と根拠

ORDレコード
ord-3e186dcac467463c850100263db0234b
出典データセット
uspto-grants-1999_02
特許番号
US05866589

反応ノート

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