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Chloroacetyl chloride → 3-(1-cyano-1-methylethyl)-N-{3-[(7-cyano-2-{[(4-methylpiperazin-1-yl)acetyl]amino}-1,3-benzothiazol-6-yl)oxy]phenyl}benzamide

HRID 455164
ノート
印刷プレビュー

反応式

HRID 455164 の反応式
[NH2:1][C:2]1[S:3][C:4]2[C:10]([C:11]#[N:12])=[C:9]([O:13][C:14]3[CH:15]=[C:16]([NH:20][C:21](=[O:33])[C:22]4[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([C:31]#[N:32])([CH3:30])[CH3:29])[CH:23]=4)[CH:17]=[CH:18][CH:19]=3)[CH:8]=[CH:7][C:5]=2[N:6]=1.Cl[CH2:35][C:36](Cl)=[O:37].C(=O)([O-])O.[Na+].C(N(CC)CC)C.[CH3:51][N:52]1[CH2:57][CH2:56][NH:55][CH2:54][CH2:53]1>CN(C)C(=O)C.C(OCC)(=O)C>[C:31]([C:28]([C:24]1[CH:23]=[C:22]([CH:27]=[CH:26][CH:25]=1)[C:21]([NH:20][C:16]1[CH:17]=[CH:18][CH:19]=[C:14]([O:13][C:9]2[CH:8]=[CH:7][C:5]3[N:6]=[C:2]([NH:1][C:36](=[O:37])[CH2:35][N:55]4[CH2:56][CH2:57][N:52]([CH3:51])[CH2:53][CH2:54]4)[S:3][C:4]=3[C:10]=2[C:11]#[N:12])[CH:15]=1)=[O:33])([CH3:30])[CH3:29])#[N:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 531671-MethylpiperazineHCID 516892Sodium BicarbonateHCID 86644680N-{3-[(2-amino-7-cyano-1,3-benzothiazol-6-yl)oxy]phenyl}-3-(1-cyano-1-methylethyl)benzamide

生成物 1

HCID 59454510
3-(1-cyano-1-methylethyl)-N-{3-[(7-cyano-2-{[(4-methylpiperazin-1-yl)acetyl]amino}-1,3-benzothiazol-6-yl)oxy]phenyl}benzamide
収率 64.3%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 31374Dimethylacetamide溶媒

実験手順

To a solution of N-{3-[(2-amino-7-cyano-1,3-benzothiazol-6-yl)oxy]phenyl}-3-(1-cyano-1-methylethyl)benzamide (150 mg, 0.33 mmol) produced in Example 1 (iv) in N,N-dimethylacetamide (3 mL) was added chloroacetyl chloride (58 μL, 0.73 mmol), and the mixture was stirred at room temperature for 2 hr. 5% Aqueous sodium hydrogen carbonate solution (10 mL) was added to the reaction mixture, and the mixture was extracted with ethyl acetate (10 mL). The extract was washed with saturated brine (10 ml), and dried over anhydrous sodium sulfate. Insoluble material was filtered off, the filtrate was concentrated under reduced pressure, the obtained residue was dissolved in tetrahydrofuran (3 mL). Triethylamine (136 μL, 0.99 mmol) and 1-methylpiperazine (110 μL, 0.99 mmol) were added to the mixture, and the mixture was stirred at 80° C. for 8 hr. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (10 mL), washed successively with water (10 mL) and saturated brine (10 mL), and dried over anhydrous sodium sulfate. Insoluble material was filtered off, the filtrate was concentrated under reduced pressure, and the obtained residue was purified by basic silica gel column chromatography (methanol/ethyl acetate=0/100→15/85). The obtained solution was concentrated under reduced pressure. The residue was crystallized from ethyl acetate/diisopropyl ether to give the title compound (126 mg, 64%) as a white powder.

後処理

  1. extractionthe mixture was extracted with ethyl acetate (10 mL)
  2. washThe extract was washed with saturated brine (10 ml)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationInsoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. dissolutionthe obtained residue was dissolved in tetrahydrofuran (3 mL)
  7. stirringthe mixture was stirred at 80° C. for 8 hr
  8. temperatureThe reaction mixture was cooled to room temperature
  9. washwashed successively with water (10 mL) and saturated brine (10 mL)
  10. dry with materialdried over anhydrous sodium sulfate
  11. filtrationInsoluble material was filtered off
  12. concentrationthe filtrate was concentrated under reduced pressure
  13. customthe obtained residue was purified by basic silica gel column chromatography (methanol/ethyl acetate=0/100→15/85)
  14. concentrationThe obtained solution was concentrated under reduced pressure
  15. customThe residue was crystallized from ethyl acetate/diisopropyl ether

出典と根拠

ORDレコード
ord-93c65eba8c5e4ef4a2e04655e6337a72
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08497274B2

反応ノート

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