Tetrahydrofuran → [5-Ethyl-6-(furan-2-yl)-pyrimidin-4-yl]-hydrazine

HRID 1527641ノート

反応式

HRID 1527641 の反応式
Cl[C:2]1[C:7]([CH2:8][CH3:9])=[C:6]([C:10]2[O:11][CH:12]=[CH:13][CH:14]=2)[N:5]=[CH:4][N:3]=1.O.[NH2:16][NH2:17].C(N(CC)CC)C.C1COCC1>O>[CH2:8]([C:7]1[C:2]([NH:16][NH2:17])=[N:3][CH:4]=[N:5][C:6]=1[C:10]1[O:11][CH:12]=[CH:13][CH:14]=1)[CH3:9]

参加物

6

反応物 4

HCID 8028TetrahydrofuranHCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)2 回HCID 656454164-Chloro-5-ethyl-6-(furan-2-yl)-pyrimidine

生成物 1

HCID 67814467[5-Ethyl-6-(furan-2-yl)-pyrimidin-4-yl]-hydrazine収率 97.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 4-chloro-5-ethyl-6-(furan-2-yl)-pyrimidine (3.0 g), hydrazine monohydrate (3.0 g), triethylamine (3.0 g), and THF (20 ml) was stirred under reflux for 2 hours. To the mixture, hydrazine monohydrate (1 g) was added, and stirred under reflux for 3 hours. After standing to cool the reaction mixture to room temperature, to the reaction mixture, water was added, and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure to give 2.85 g of [5-ethyl-6-(furan-2-yl)-pyrimidin-4-yl]-hydrazine.

後処理

  1. temperatureunder reflux for 2 hours
  2. stirringstirred
  3. temperatureunder reflux for 3 hours
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-19306e042661451f8b644e57485b585c
出典データセット
uspto-grants-2015_07
特許番号
US09089136B2

反応ノート

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