Stannous Chloride → 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one

HRID 354739ノート

反応式

HRID 354739 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-])=O)[CH:17]=[CH:18][C:13]=2[N:12]([CH3:22])[C:11](=[O:23])[C:10]([CH3:25])([CH3:24])[N:9]=1.[Sn](Cl)Cl>Cl>[NH2:19][C:16]1[CH:17]=[CH:18][C:13]2[N:12]([CH3:22])[C:11](=[O:23])[C:10]([CH3:25])([CH3:24])[N:9]=[C:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[F:1])[C:14]=2[CH:15]=1

参加物

4

反応物 2

HCID 24479Stannous ChlorideHCID 205061565-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one

生成物 1

HCID 205061627-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

1.5 g (0.0044 mol) of 5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one are dissolved in 15 ml of concentrated hydrochloric acid, treated with 3.3 g of tin (II) chloride and stirred at room temperature for 15 minutes. The reaction mixture is poured into a mixture of ice and soda solution and extracted with methylene chloride. After drying and evaporating the organic phase, the residue is recrystallised from ether. There is obtained 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one of melting point 190°-191°.

後処理

  1. additionThe reaction mixture is poured into a mixture of ice and soda solution
  2. extractionextracted with methylene chloride
  3. customAfter drying
  4. customevaporating the organic phase
  5. customthe residue is recrystallised from ether

出典と根拠

ORDレコード
ord-9c4fbeafa6ab4ef5964d0c5a7b80fc0d
出典データセット
uspto-grants-1983_03
特許番号
US04377522

反応ノート

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