Hydrazine hydrate (1:1) → [4-(6-aminomethyl-1H-inden-2-yl)-butyl]-dipropyl-amine

HRID 2080740ノート

反応式

HRID 2080740 の反応式
[CH2:1]([N:4]([CH2:28][CH2:29][CH3:30])[CH2:5][CH2:6][CH2:7][CH2:8][C:9]1[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[C:14]([CH2:18][N:19]3C=C4C(C=CC=C4)=C3)[CH:15]=2)[CH:10]=1)[CH2:2][CH3:3].O.NN>CO>[NH2:19][CH2:18][C:14]1[CH:15]=[C:16]2[C:11]([CH:10]=[C:9]([CH2:8][CH2:7][CH2:6][CH2:5][N:4]([CH2:28][CH2:29][CH3:30])[CH2:1][CH2:2][CH3:3])[CH2:17]2)=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 866149102-[2-(4-dipropylamino-butyl)-3H-inden-5-ylmethyl]-isoindol

生成物 1

HCID 23155401[4-(6-aminomethyl-1H-inden-2-yl)-butyl]-dipropyl-amine収率 65.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

The compound (82.0 mg) obtained in Example 11-12 was dissolved in methanol (4.1 ml) and added with hydrazine monohydrate (0.082 ml) and the whole was refluxed under heating for 3 hours. The reaction solution was concentrated under reduced pressure. Then, the residue was added with water and subjected to extraction with chloroform. The organic layer was washed with a saturated saline solution, dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate), thereby obtaining the subject compound (40.1 mg) as a yellow oily substance.

後処理

  1. temperaturethe whole was refluxed
  2. temperatureunder heating for 3 hours
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. additionThen, the residue was added with water
  5. extractionsubjected to extraction with chloroform
  6. washThe organic layer was washed with a saturated saline solution
  7. dry with materialdried with anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified through silica gel column chromatography (chloroform/ethyl acetate)

出典と根拠

ORDレコード
ord-c13f1557c993480daa9715a205cd9c4c
出典データセット
uspto-grants-2011_04
特許番号
US07932281B2

反応ノート

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