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

HRID 1527641노트

반응식

HRID 1527641 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-19306e042661451f8b644e57485b585c
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09089136B2

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