Water → 5-(2-fluorophenyl)-7-nitro-3H-1,4-benzodiazepine-2(1H)-thione

HRID 566291

反応式

HRID 566291 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=O)[CH2:10][N:9]=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:32])=CC=1.C(=O)([O-])O.[Na+].O>CN(C)P(=O)(N(C)C)N(C)C>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[S:32])[CH2:10][N:9]=1

参加物

6

反応物 4

HCID 962WaterHCID 87949Lawesson's reagentHCID 516892Sodium BicarbonateHCID 520217Norflunitrazepam

生成物 1

HCID 123714345-(2-fluorophenyl)-7-nitro-3H-1,4-benzodiazepine-2(1H)-thione収率 183.2%

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

反応条件

温度
105 °C

実験手順

A solution of 20.0 g of 5-(2-fluorophenyl)-7-nitro-3H-1,4-benzodiazepin-2(1H)-one (G. M. Clarke, J. B. Lee, F. J. Swinbourne & B. Williamson, J. Chem. Res. Synop. 1980, 400) in 100 ml of hexamethylphosphoric acid triamide was treated with 14 g of Lawesson reagent and the mixture was stirred at 105° C. for 70 min. The reaction mixture was poured into 800 ml of saturated aqueous sodium hydrogen carbonate solution and 800 ml of water. After stirring at room temperature for 15 min. the precipitate was filtered off, washed with water and dried. There were obtained 20 g of crude 5-(2-fluorophenyl)-7-nitro-3H-1,4-benzodiazepine-2(1H)-thione, which was used in this form for the next step.

後処理

  1. stirringAfter stirring at room temperature for 15 min. the precipitate
  2. filtrationwas filtered off
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-431e21bd542f4c30ad9c362f519203d0
出典データセット
uspto-grants-2001_01
特許番号
US06174881B1

関連ノート

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