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

HRID 566272
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HRID 566272 반응식
[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
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참가 물질

3

반응물 1

HCID 21265977HCID 21265977, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.).

후처리

  • 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
  • 출처 및 근거

    ORD 기록
    ord-6558805d5fed41a9afbab82b6dfa0720
    출처 데이터셋
    uspto-grants-2001_01
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US06174881B1

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