Hydrazine → HCID 57515603, 화합물

HRID 1469340노트

반응식

HRID 1469340 반응식
NN.[NH2:3][C:4]1[C:13]2[N:14]=[C:15]([CH2:23][N:24]3C(=O)C4C(=CC=CC=4)C3=O)[N:16]([CH2:17][C:18]3([OH:22])[CH2:21][CH2:20][CH2:19]3)[C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[N:5]=1>C(O)C>[NH2:3][C:4]1[C:13]2[N:14]=[C:15]([CH2:23][NH2:24])[N:16]([CH2:17][C:18]3([OH:22])[CH2:21][CH2:20][CH2:19]3)[C:12]=2[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[N:5]=1

참가 물질

4

반응물 2

HCID 9321HydrazineHCID 57515602HCID 57515602, 화합물

생성물 1

HCID 57515603HCID 57515603, 화합물수율 59.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Under a nitrogen atmosphere, hydrazine (0.89 mL, 28 mmol) was added to a suspension of 2-({4-amino-1-[(1-hydroxycyclobutyl)methyl]-1H-imidazo[4,5-c]quinolin-2-yl}methyl)-1H-isoindole-1,3(2H)-dione (2.42 g, 5.66 mmol) in ethanol (57 mL), and the reaction was stirred for two hours at room temperature. The ethanol was removed under reduced pressure, and the resulting white solid was triturated with 2 N hydrochloric acid. The resulting suspension was filtered to remove a solid, and the filter cake was washed with water. The filtrate was made basic with the addition of solid sodium bicarbonate. A precipitate formed and was isolated by filtration, washed with water, and dried at 50° C. for three days in a vacuum oven to provide 0.994 g of 1-{[4-amino-2-(aminomethyl)-1H-imidazo[4,5-c]quinolin-1-yl]methyl}cyclobutanol as a yellow solid.

후처리

  1. customThe ethanol was removed under reduced pressure
  2. customthe resulting white solid was triturated with 2 N hydrochloric acid
  3. filtrationThe resulting suspension was filtered
  4. customto remove a solid
  5. washthe filter cake was washed with water
  6. additionThe filtrate was made basic with the addition of solid sodium bicarbonate
  7. customA precipitate formed
  8. customwas isolated by filtration
  9. washwashed with water
  10. customdried at 50° C. for three days in a vacuum oven

출처 및 근거

ORD 기록
ord-722cd49dd8f24bfdb2a6bdae481889dc
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006264B2

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