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Water → 12-amino-3-fluoro-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine

HRID 1281819
ノート
印刷プレビュー

反応式

HRID 1281819 の反応式
[Sn](Cl)Cl.[F:4][C:5]1[CH:6]=[CH:7][C:8]2[C:12]([C:13]#[N:14])=[C:11]([NH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[N+:22]([O-])=O)[S:10][C:9]=2[CH:25]=1.O>Cl.C(O)C>[NH2:14][C:13]1[C:12]2[C:8]3[CH:7]=[CH:6][C:5]([F:4])=[CH:25][C:9]=3[S:10][C:11]=2[NH:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[N:22]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 24479Stannous ChlorideHCID 184221416-Fluoro-2-(2-nitroanilino)benzo[b]thiophene-3-carbonitrile

生成物 1

HCID 13581640212-amino-3-fluoro-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine収率 82.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 702
Ethanol
溶媒

反応条件

温度
50 °C

実験手順

Tin(II) chloride (50 g) was dissolved in a 18% hydrochloric acid (250 ml) solution heated to 50° C., and a suspension of 6-fluoro-2-(2-nitroanilino)benzo[b]thiophene-3-carbonitrile (20 g) in ethanol (280 ml) was added. The mixture was refluxed under heating for 4 hours. Then, the reaction mixture was cooled to 40° C. and poured into water (1 L) and the mixture was stood still for 30 minutes. The precipitated crystals were filtered by suction and washed with water (500 ml) to give 12-amino-3-fluoro-6H-[1]benzothieno[2,3-b][1,5]benzodiazepine 1 hydrochloride (15 g).

後処理

  1. additionwas added
  2. temperatureThe mixture was refluxed
  3. temperatureunder heating for 4 hours
  4. temperatureThen, the reaction mixture was cooled to 40° C.
  5. filtrationThe precipitated crystals were filtered by suction
  6. washwashed with water (500 ml)

出典と根拠

ORDレコード
ord-8cb91432698e408f807595f845aa7913
出典データセット
uspto-grants-2002_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06455521B1

反応ノート

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