Hydrazine → 2-(2-aminoethyl)-6-phenylpyridazin-3(2H)-one

HRID 1878742ノート

反応式

HRID 1878742 の反応式
[O:1]=[C:2]1[N:7]([CH2:8][CH2:9][N:10]2C(=O)C3C(=CC=CC=3)C2=O)[N:6]=[C:5]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:4]=[CH:3]1.NN>CO>[NH2:10][CH2:9][CH2:8][N:7]1[C:2](=[O:1])[CH:3]=[CH:4][C:5]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[N:6]1

参加物

4

反応物 2

HCID 9321HydrazineHCID 13103521HCID 13103521、化合物

生成物 1

HCID 129026032-(2-aminoethyl)-6-phenylpyridazin-3(2H)-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
75 °C

実験手順

A mixture of 2-(2-(6-oxo-3-phenylpyridazin-1(6H)-yl)ethyl)isoindoline-1,3-dione (2.1 g, 6.1 mmol) and hydrazine (10 mL, 10.0 mmol) (THF) in MeOH (40 mL) was heated to 75° C. A clear solution was formed. After overnight (18 h), the slurry was cooled to room temperature and was filtered and washed with MeOH. The filtrate was concentrated and washed with 20% MeOH/CH2Cl2 to give a yellow solid (LCMS indicated the presence of product). The filtrate was concentrated under vacuum and was carried to next step.

後処理

  1. customA clear solution was formed
  2. temperaturethe slurry was cooled to room temperature
  3. filtrationwas filtered
  4. washwashed with MeOH
  5. concentrationThe filtrate was concentrated
  6. washwashed with 20% MeOH/CH2Cl2
  7. customto give a yellow solid (LCMS
  8. concentrationThe filtrate was concentrated under vacuum

出典と根拠

ORDレコード
ord-06085f8a8f524b67a71ae8284e771fcb
出典データセット
uspto-grants-2012_11
特許番号
US08314087B2

反応ノート

読み込み中…