Water → 4-(4-Aminophenoxy)-2-butylaminopyridine

HRID 387791노트

반응식

HRID 387791 반응식
[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([NH:13][C:14](=O)[CH2:15][CH2:16][CH3:17])[CH:8]=2)=[CH:4][CH:3]=1.[H-].[Li+].[Al+3].[H-].[H-].[H-].O>O1CCCC1>[NH2:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([NH:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH:8]=2)=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 229364634-(4-Aminophenoxy)-2-butyrylaminopyridine

생성물 1

HCID 229369234-(4-Aminophenoxy)-2-butylaminopyridine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

After dissolving 80 mg of 4-(4-aminophenoxy)-2-butyrylaminopyridine in 8 ml of tetrahydrofuran, 67 mg of aluminum lithium hydride was added while stirring at room temperature, and the mixture was stirred at 70° C. for 10 minutes. Water was added, extraction was performed with ethyl acetate, and then silica gel was added to the extract and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel and purified by column chromatography (ethyl acetate) to obtain 54 mg of the target substance as a brown oil.

후처리

  1. additionwas added
  2. stirringthe mixture was stirred at 70° C. for 10 minutes
  3. extractionextraction
  4. additionsilica gel was added to the
  5. extractionextract
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionThe silica gel was charged into a dry column
  8. custompurified by column chromatography (ethyl acetate)
  9. customto obtain 54 mg of the target substance as a brown oil

출처 및 근거

ORD 기록
ord-f220f6643bf34d84be796c82d8132202
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372981B2

반응 노트

불러오는 중…