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Bromine → N-{3-[(2-amino[1,3]thiazolo[5,4-b]pyridin-5-yl)oxy]-4-cyanophenyl}-3-(1-cyano-1-methylethyl)benzamide

HRID 1800491
ノート
印刷プレビュー

反応式

HRID 1800491 の反応式
[S-:1][C:2]#[N:3].[K+].[NH2:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][C:13]2[CH:14]=[C:15]([NH:21][C:22](=[O:34])[C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([C:32]#[N:33])([CH3:31])[CH3:30])[CH:24]=3)[CH:16]=[CH:17][C:18]=2[C:19]#[N:20])=[N:10][CH:11]=1.BrBr>C(O)(=O)C>[NH2:3][C:2]1[S:1][C:11]2[C:6]([N:5]=1)=[CH:7][CH:8]=[C:9]([O:12][C:13]1[CH:14]=[C:15]([NH:21][C:22](=[O:34])[C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([C:29]([C:32]#[N:33])([CH3:31])[CH3:30])[CH:24]=3)[CH:16]=[CH:17][C:18]=1[C:19]#[N:20])[N:10]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24408BromineHCID 516872Potassium thiocyanateHCID 68418578N-{3-[(5-aminopyridin-2-yl)oxy]-4-cyanophenyl}-3-(1-cyano-1-methylethyl)benzamide

生成物 1

HCID 86646007N-{3-[(2-amino[1,3]thiazolo[5,4-b]pyridin-5-yl)oxy]-4-cyanophenyl}-3-(1-cyano-1-methylethyl)benzamide収率 81.3%

試薬・触媒・溶媒 1

HCID 176Acetic Acid
溶媒
3 回

実験手順

Potassium thiocyanate (536 mg, 5.52 mmol) was suspended in acetic acid (10 mL), and the mixture was stirred at room temperature for 10 min. A solution of N-{3-[(5-aminopyridin-2-yl)oxy]-4-cyanophenyl}-3-(1-cyano-1-methylethyl)benzamide (550 mg, 1.38 mmol) in acetic acid (10 mL) was added to the obtained solution, and the mixture was further stirred at room temperature for 10 min. A solution of bromine (242 mg, 1.51 mmol) in acetic acid (7 mL) was slowly added dropwise to the obtained solution. After the completion of the dropwise addition, the mixture was stirred at room temperature for 12 hr. The yielded yellow insoluble material was filtered off, and washed with acetic acid. The filtrate and the washing fluid were combined, and concentrated under reduced pressure. The obtained residue was suspended in ethyl acetate (100 mL), and the suspension was washed with 5% aqueous sodium hydrogen carbonate solution (100 mL) and saturated brine (100 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/50→0/100). The obtained solution was concentrated under reduced pressure to give the title compound (0.51 g, 81%) as a pale-yellow amorphous substance.

後処理

  1. stirringthe mixture was further stirred at room temperature for 10 min
  2. additionAfter the completion of the dropwise addition
  3. stirringthe mixture was stirred at room temperature for 12 hr
  4. filtrationThe yielded yellow insoluble material was filtered off
  5. washwashed with acetic acid
  6. concentrationconcentrated under reduced pressure
  7. washthe suspension was washed with 5% aqueous sodium hydrogen carbonate solution (100 mL) and saturated brine (100 mL)
  8. dry with materialdried over anhydrous sodium sulfate
  9. filtrationThe insoluble material was filtered off
  10. concentrationthe filtrate was concentrated under reduced pressure
  11. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate=50/50→0/100)
  12. concentrationThe obtained solution was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b0eb1c3b22a64ac49108abb76f9e57f3
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08344135B2

反応ノート

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