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Tetrabutylammonium Fluoride → (2S)-2-(1-(2-chlorophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-(2-hydroxyethoxy)-N-(pyridin-2-yl)propanamide

HRID 1098047
ノート
印刷プレビュー

反応式

HRID 1098047 の反応式
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Si]([O:36][CH2:37][CH2:38][O:39][CH2:40][C@H:41]([O:51][C:52]1[N:57]=[CH:56][N:55]=[C:54]2[N:58]([C:61]3[CH:66]=[CH:65][CH:64]=[CH:63][C:62]=3[Cl:67])[N:59]=[CH:60][C:53]=12)[C:42]([NH:44][C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][N:46]=1)=[O:43])(C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1>O1CCCC1>[Cl:67][C:62]1[CH:63]=[CH:64][CH:65]=[CH:66][C:61]=1[N:58]1[C:54]2=[N:55][CH:56]=[N:57][C:52]([O:51][C@@H:41]([CH2:40][O:39][CH2:38][CH2:37][OH:36])[C:42]([NH:44][C:45]3[CH:50]=[CH:49][CH:48]=[CH:47][N:46]=3)=[O:43])=[C:53]2[CH:60]=[N:59]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 2724141Tetrabutylammonium FluorideHCID 57504548(2S)-3-(2-(tert-butyldiphenylsilyloxy)ethoxy)-2-(1-(2-chlorophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-N-(pyridin-2-yl)propanamide

生成物 1

HCID 57504429(2S)-2-(1-(2-chlorophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-3-(2-hydroxyethoxy)-N-(pyridin-2-yl)propanamide収率 75.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of tetrabutylammonium fluoride (1M in THF) (0.984 mL, 0.98 mmol) was added in one portion to a stirred solution of (2S)-3-(2-(tert-butyldiphenylsilyloxy)ethoxy)-2-(1-(2-chlorophenyl)-1H-pyrazolo[3,4-d]pyrimidin-4-yloxy)-N-(pyridin-2-yl)propanamide (Intermediate AQ5) (0.682 g, 0.98 mmol) in tetrahydrofuran (15 mL). The resulting solution was stirred at ambient temperature for 30 minutes. The reaction mixture was quenched with saturated NH4Cl (10 mL), and diluted with water (20 mL) and EtOAc (50 mL). The organic layer was separated and the aqueous layer extracted with EtOAc (50 mL), The combined organics were dried (MgSO4), filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 80 to 100% EtOAc in isohexane to afford the product (0.335 g, 74.9%). 1H NMR: (400 MHz, CDCl3) δ 2.91 (1H, s), 3.74-3.79 (4H, m), 4.15-4.25 (2H, m), 6.10 (1H, t), 7.06-7.10 (1H, m), 7.45-7.63 (4H, m), 7.71-7.75 (1H, m), 8.19 (1H, d), 8.27-8.29 (1H, m), 8.44 (1H, s), 8.60 (1H, s), 9.01 (1H, s); m/z (ES+) (M+H)+=455; HPLC tR=1.76 min.

後処理

  1. customThe reaction mixture was quenched with saturated NH4Cl (10 mL)
  2. additiondiluted with water (20 mL) and EtOAc (50 mL)
  3. customThe organic layer was separated
  4. extractionthe aqueous layer extracted with EtOAc (50 mL)
  5. dry with materialThe combined organics were dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. customto afford crude product
  9. customThe crude product was purified by flash silica chromatography, elution gradient 80 to 100% EtOAc in isohexane

出典と根拠

ORDレコード
ord-faa5cd5ce07b4e819dac1458c8841d32
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08143263B2

反応ノート

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