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HCID 21265977、化合物 → 5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine

HRID 566272
ノート
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反応式

HRID 566272 の反応式
[NH2:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[F:18])=[N:8][CH2:9][C:10]#[N:11]>C(O)(=O)C>[F:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7]1[C:6]2[CH:5]=[CH:4][S:3][C:2]=2[N:1]=[C:10]([NH2:11])[CH2:9][N:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 21265977HCID 21265977、化合物

生成物 1

HCID 212660085-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine収率 24.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 70 g of [(2-amino-thiophen-3-yl)-(2-fluoro-phenyl)-methyleneamino]acetonitrile in 980 ml of acetic acid was stirred at 65° C. under argon for 1.5 h. After cooling the solvent was removed in a vacuum, the residue was dissolved in dichloromethane and neutralized with sodium bicarbonate solution while cooling with ice and extracted. The dichloromethane extracts were dried with sodium sulphate, filtered and evaporated to dryness in a vacuum. After crystallization from dichloromethane there were obtained 17.1 g of 5-(2-fluoro-phenyl)-3H-thieno[2,3-e][1,4]diazepin-2-ylamine of m.p. 219-220° C. (dec.).

後処理

  • temperatureAfter cooling the solvent
  • customwas removed in a vacuum
  • dissolutionthe residue was dissolved in dichloromethane and neutralized with sodium bicarbonate solution
  • temperaturewhile cooling with ice
  • extractionextracted
  • dry with materialThe dichloromethane extracts were dried with sodium sulphate
  • filtrationfiltered
  • customevaporated to dryness in a vacuum
  • customAfter crystallization from dichloromethane
  • 出典と根拠

    ORDレコード
    ord-6558805d5fed41a9afbab82b6dfa0720
    出典データセット
    uspto-grants-2001_01
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US06174881B1

    反応ノート

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