Hydrazine hydrate (1:1) → 4-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)piperazin-1-yl]-butylamine

HRID 219699ノート

反応式

HRID 219699 の反応式
[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:13][CH2:12]2)[CH:8]=[C:7]([CH:32]2[CH2:35][CH2:34][CH2:33]2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([C:5]1[N:10]=[C:9]([N:11]2[CH2:12][CH2:13][N:14]([CH2:17][CH2:18][CH2:19][CH2:20][NH2:21])[CH2:15][CH2:16]2)[CH:8]=[C:7]([CH:32]2[CH2:35][CH2:34][CH2:33]2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 690260812-{4-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butyl}-isoindole-1,3-dione

生成物 1

HCID 690260674-[4-(2-tert-Butyl-6-cyclobutyl-pyrimidin-4-yl)piperazin-1-yl]-butylamine収率 68.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2.4 g of 2-{4-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-butyl}-isoindole-1,3-dione (5.05 mmol) and 1.0 g of hydrazine hydrate (20.2 mmol) were dissolved in 20 ml of ethanol and heated to reflux for 1 h. The precipitate was filtered and the filtrate extracted with water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, and concentrated to dryness to yield 1.2 g of the title compound.

後処理

  1. temperatureheated
  2. temperatureto reflux for 1 h
  3. filtrationThe precipitate was filtered
  4. extractionthe filtrate extracted with water and ethyl acetate
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-53e301ff681744bb85772887fb338a00
出典データセット
uspto-grants-2012_06
特許番号
US08202868B2

反応ノート

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