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Hydrochloric Acid → N-[5-(3,5-difluoro-benzenesulfonyl)-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide

HRID 1640990
ノート
印刷プレビュー

反応式

HRID 1640990 の反応式
[F:1][C:2]1[CH:3]=[C:4]([S:9]([C:12]2[CH:13]=[C:14]3[C:18](=[CH:19][CH:20]=2)[N:17](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[N:16]=[C:15]3[NH:40][C:41](=[O:68])[C:42]2[CH:47]=[CH:46][C:45]([N:48]3[CH2:53][CH2:52][N:51]([CH3:54])[CH2:50][CH2:49]3)=[CH:44][C:43]=2[N:55]([CH:62]2[CH2:67][CH2:66][O:65][CH2:64][CH2:63]2)[C:56](=[O:61])[C:57]([F:60])([F:59])[F:58])(=[O:11])=[O:10])[CH:5]=[C:6]([F:8])[CH:7]=1.Cl>O1CCOCC1.CO>[F:8][C:6]1[CH:5]=[C:4]([S:9]([C:12]2[CH:13]=[C:14]3[C:18](=[CH:19][CH:20]=2)[NH:17][N:16]=[C:15]3[NH:40][C:41](=[O:68])[C:42]2[CH:47]=[CH:46][C:45]([N:48]3[CH2:49][CH2:50][N:51]([CH3:54])[CH2:52][CH2:53]3)=[CH:44][C:43]=2[N:55]([CH:62]2[CH2:67][CH2:66][O:65][CH2:64][CH2:63]2)[C:56](=[O:61])[C:57]([F:59])([F:60])[F:58])(=[O:10])=[O:11])[CH:3]=[C:2]([F:1])[CH:7]=1
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 2

HCID 313Hydrochloric AcidHCID 86643843N-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide

生成物 1

HCID 86643844N-[5-(3,5-difluoro-benzenesulfonyl)-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide収率 80%

試薬・触媒・溶媒 2

HCID 887
Methanol
溶媒
HCID 312751,4-Dioxane溶媒2 回

実験手順

A mixture of N-[5-(3,5-difluoro-benzenesulfonyl)-1-trityl-1H-indazol-3-yl]-4-(4-methyl-piperazin-1-yl)-2-[(tetrahydro-pyran-4-yl)-(2,2,2-trifluoro-acetyl)-amino]-benzamide (2.4 g, 2.53 mmol), 4N hydrochloric acid in 1,4-dioxane (35 mL), methanol (50 mL) and 1,4-dioxane (15 mL) was stirred at room temperature for 3 hours. The solvents were removed under reduced pressure and the residue dissolved in dichloromethane, washed with water, brine, dried over sodium sulfate and evaporated to dryness. The crude was purified by flash chromatography on silica gel using dichloromethane/acetone 1:1 as the eluant affording the title compound as a pale yellow solid (1.43 g, 80% yield).

後処理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with water, brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated to dryness
  6. customThe crude was purified by flash chromatography on silica gel

出典と根拠

ORDレコード
ord-271d8d91ce7f48a6aa4042483d9f611e
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08114865B2

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