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Hydrazine → HCID 68539374、化合物

HRID 1187425
ノート
印刷プレビュー

反応式

HRID 1187425 の反応式
NN.[NH2:3][C:4]1[C:13]2[N:14]=[CH:15][N:16]([CH2:17][CH2:18][CH2:19][CH2:20][O:21][N:22]3C(=O)C4C(=CC=CC=4)C3=O)[C:12]=2[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[N:5]=1>C(O)C>[NH2:22][O:21][CH2:20][CH2:19][CH2:18][CH2:17][N:16]1[C:12]2[C:11]3[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=3[N:5]=[C:4]([NH2:3])[C:13]=2[N:14]=[CH:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 9321Hydrazine2 回HCID 68539763HCID 68539763、化合物

生成物 1

HCID 68539374HCID 68539374、化合物収率 135%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Anhydrous hydrazine (94 mg, 2.96 mmol) was added to 2-[4-(4-amino-6,7,8,9-tetrahydro-1H-imidazo[4,5-c]quinolin-1-yl)butoxy]-1H-isoindole-1,3(2H)-dione (600 mg, 1.48 mmol) in ethanol (25 mL) at ambient temperature. The reaction was stirred overnight, and additional hydrazine (2 equivalents) was added. After sting for 2 hours at ambient temperature, the reaction was concentrated under reduced pressure. The residue was diluted with dichloromethane and concentrated under reduced pressure three times to remove the hydrazine and then dried under vacuum to provide 550 mg of impure 1-[4-(aminooxy)butyl]-6,7,8,9-tetrahydro-1H-imidazo[4,5-c]quinolin4-amine as an orange solid.

後処理

  1. waitAfter sting for 2 hours at ambient temperature
  2. concentrationthe reaction was concentrated under reduced pressure
  3. additionThe residue was diluted with dichloromethane
  4. concentrationconcentrated under reduced pressure three times
  5. customto remove the hydrazine
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-d8aab179250049069e08957606f36398
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673932B2

反応ノート

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