Sodium Hydroxide → 7-chloro-5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine

HRID 566273ノート

反応式

HRID 566273 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]2[CH:18]=[CH:17][S:16][C:10]=2[N:11]=[C:12]([NH2:15])[CH2:13][N:14]=1.[Cl:19]Cl.[OH-].[Na+]>CO.ClCCl>[Cl:19][C:17]1[S:16][C:10]2[N:11]=[C:12]([NH2:15])[CH2:13][N:14]=[C:8]([C:3]3[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=3[F:1])[C:9]=2[CH:18]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 212660085-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine

生成物 1

HCID 212660107-chloro-5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒2 回

実験手順

19 g of 5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine were dissolved in 730 ml of 5% methanol in dichloromethane, treated while stirring well with 327 g of a 2.8% solution of chlorine gas in 5% methanol in dichloromethane and stirred at room temperature under argon for 5 minutes. Thereafter, the reaction mixture was poured into 600 ml of 0.2N sodium hydroxide solution while cooling with ice and extracted. The dichloromethane extracts were dried with sodium sulphate, filtered and the solvent was evaporated in a vacuum. After two fold boiling of the residue in 5% methanol in dichloromethane and filtration there were obtained 7.4 g of 7-chloro-5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine of m.p. 215-217° C. (dec.).

後処理

  1. additiontreated
  2. temperaturewhile cooling with ice
  3. extractionextracted
  4. dry with materialThe dichloromethane extracts were dried with sodium sulphate
  5. filtrationfiltered
  6. customthe solvent was evaporated in a vacuum
  7. filtrationAfter two fold boiling of the residue in 5% methanol in dichloromethane and filtration there

出典と根拠

ORDレコード
ord-8836ab4bc7014ac48c683773645a7f18
出典データセット
uspto-grants-2001_01
特許番号
US06174881B1

反応ノート

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