Hydrazine → HCID 57515603、化合物

HRID 44799ノート

反応式

HRID 44799 の反応式
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

参加物

4

反応物 2

HCID 9321HydrazineHCID 57515602HCID 57515602、化合物

生成物 1

HCID 57515603HCID 57515603、化合物収率 59.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-03e00ae7817945c39f20c03923f2b37c
出典データセット
uspto-grants-2013_09
特許番号
US08541438B2

反応ノート

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