Hydrazine hydrate (1:1) → HCID 178526552、化合物

HRID 385742ノート

反応式

HRID 385742 の反応式
C[N:2](/[CH:4]=[N:5]/[C:6]([C:8]1[S:9][C:10]([N+:13]([O-:15])=[O:14])=[CH:11][CH:12]=1)=O)C.O.[NH2:17]N>CC(O)=O>[N+:13]([C:10]1[S:9][C:8]([C:6]2[N:5]=[CH:4][NH:2][N:17]=2)=[CH:12][CH:11]=1)([O-:15])=[O:14]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 178484334HCID 178484334、化合物

生成物 1

HCID 178526552HCID 178526552、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

N-[(1E)-(Dimethylamino)methylene]-5-nitrothiophene-2-carboxamide (7.00 g, 30.8 mmol) was combined with AcOH (70 mL) and hydrazine hydrate (65% wt, 2.76 mL, 37.0 mmol) and stirred at 90° C. for 1.5 h. The yellow solution was cooled to room temperature and concentrated. The resulting slurry was diluted with CH2Cl2 and saturated NaHCO3 and stirred. The yellow precipitate was isolated by filtration and dried to provide the title compound as a yellow solid.

後処理

  1. temperatureThe yellow solution was cooled to room temperature
  2. concentrationconcentrated
  3. additionThe resulting slurry was diluted with CH2Cl2 and saturated NaHCO3
  4. stirringstirred
  5. customThe yellow precipitate was isolated by filtration
  6. customdried

出典と根拠

ORDレコード
ord-b36b9329cb3545db8ca49daa2f1197f4
出典データセット
uspto-grants-2013_02
特許番号
US08367706B2

反応ノート

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