Ethanol → 2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethanamine

HRID 1621102ノート

反応式

HRID 1621102 の反応式
[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][N:9]2C(=O)C3C(=CC=CC=3)C2=O)=[N:5][C:4]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[N:3]1.CCO>CN>[CH3:1][N:2]1[C:6]([CH2:7][CH2:8][NH2:9])=[N:5][C:4]([C:20]2[CH:25]=[CH:24][N:23]=[CH:22][CH:21]=2)=[N:3]1

参加物

4

反応物 2

HCID 702Ethanol2 回HCID 712792712-(2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethyl)isoindoline-1,3-dione

生成物 1

HCID 712792862-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethanamine収率 74.2%

試薬・触媒・溶媒 1

HCID 6329Methylamine溶媒2 回

実験手順

2-(2-(1-Methyl-3-(pyridin-4-yl)-1H-1,2,4-triazol-5-yl)ethyl)isoindoline-1,3-dione (114.9 mg, 345 μmol) was dissolved in methylamine solution in EtOH (3.07 mL, 22.5 mmol) and stirred at RT for 1 h. The reaction mixture was evaporated to give light brown solid. The solid was again dissolved in methylamine solution in EtOH (3.07 mL, 22.5 mmol) and the mixture was heated to 50° C. and stirred for 3 h. All volatiles were removed in vacuo and the residue was suspended in dichloromethane (1.5 mL) and filtered. The filtrate was evaporated to give the product as light yellow solid (81.3 mg (80% purity), 256 μmol, 74.2%) which was used without purification for the next step. MS: M=204.2 (M+H)+

後処理

  1. customThe reaction mixture was evaporated
  2. customto give light brown solid
  3. temperaturethe mixture was heated to 50° C.
  4. stirringstirred for 3 h
  5. customAll volatiles were removed in vacuo
  6. filtrationfiltered
  7. customThe filtrate was evaporated

出典と根拠

ORDレコード
ord-2aa591603db545b990db7cbae8398156
出典データセット
uspto-grants-2014_07
特許番号
US08772510B2

反応ノート

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