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Trifluoroacetic acid → N-{4-Methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-3-(pentafluoro-lambda6-sulphanyl)-5-(piperazin-1-yl)benzamide

HRID 1055702
ノート
印刷プレビュー

反応式

HRID 1055702 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[CH:12]=[C:13]([N:23]3[CH2:28][CH2:27][N:26](C(OC(C)(C)C)=O)[CH2:25][CH2:24]3)[CH:14]=[C:15]([S:17]([F:22])([F:21])([F:20])([F:19])[F:18])[CH:16]=2)=[O:10])=[CH:4][C:3]=1[N:36]1[C:43]2[N:39]([N:40]=[C:41]([C:44]3[CH:45]=[N:46][NH:47][CH:48]=3)[CH:42]=2)[CH:38]=[CH:37]1.FC(F)(F)C(O)=O>C(Cl)Cl>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9](=[O:10])[C:11]2[CH:12]=[C:13]([N:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)[CH:14]=[C:15]([S:17]([F:20])([F:22])([F:21])([F:18])[F:19])[CH:16]=2)=[CH:4][C:3]=1[N:36]1[C:43]2[N:39]([N:40]=[C:41]([C:44]3[CH:45]=[N:46][NH:47][CH:48]=3)[CH:42]=2)[CH:38]=[CH:37]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 136409111tert-Butyl 4-[3-({4-methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-carbamoyl)-5-(pentafluoro-lambda6-sulphanyl)phenyl]piperazin-1-carboxylate

生成物 1

HCID 136409110N-{4-Methyl-3-[6-(1H-pyrazol-4-yl)-1H-imidazo[1,2-b]pyrazol-1-yl]phenyl}-3-(pentafluoro-lambda6-sulphanyl)-5-(piperazin-1-yl)benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane
溶媒

実験手順

210 mg (0.19 mmol, purity 61%) of the compound from Example 47A were stirred in 4.4 ml of a 25% strength solution of trifluoroacetic acid in methylene chloride at RT for 30 min. The mixture was then concentrated under reduced pressure. The residue was dissolved in a little methanol and added to semiconcentrated aqueous sodium bicarbonate solution. After 15 min of stirring at RT, 15 ml of ethyl acetate were added. The precipitate formed was filtered off, and the organic phase of the filtrate was separated off, washed with water, dried over sodium sulphate, filtered and concentrated. Drying of the residue under reduced pressure gave 41 mg (37% of theory) of the title compound.

後処理

  1. concentrationThe mixture was then concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in a little methanol
  3. additionadded to semiconcentrated aqueous sodium bicarbonate solution
  4. addition15 ml of ethyl acetate were added
  5. customThe precipitate formed
  6. filtrationwas filtered off
  7. customthe organic phase of the filtrate was separated off
  8. washwashed with water
  9. dry with materialdried over sodium sulphate
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customDrying of the residue under reduced pressure

出典と根拠

ORDレコード
ord-89c74c610bef4dbaa8cd5e603a6fad34
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394309B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート