ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Formic Acid → 4-[2-[[(3R,3aR,6R,6aR)-3-hydroxy-2,3,3a,5,6,6a-hexahydro-furo[3,2-b]furan-6-yl]oxy]-6-chloro-1H-imidazo[4,5-b]pyridin-5-yl]benzonitrile

HRID 929194
ノート
印刷プレビュー

反応式

HRID 929194 の反応式
[OH:1][C@@H:2]1[CH2:6][O:5][C@@H:4]2[C@H:7]([O:10][C:11]3[N:12](COCC[Si](C)(C)C)[C:13]4[C:14]([N:28]=3)=[N:15][C:16]([C:20]3[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[CH:22][CH:21]=3)=[C:17]([Cl:19])[CH:18]=4)[CH2:8][O:9][C@H:3]12.C(O)=O.OS([O-])(=O)=O.[K+].[OH-].[Na+].Cl>>[OH:1][C@@H:2]1[CH2:6][O:5][C@@H:4]2[C@H:7]([O:10][C:11]3[NH:12][C:13]4[C:14]([N:28]=3)=[N:15][C:16]([C:20]3[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[CH:22][CH:21]=3)=[C:17]([Cl:19])[CH:18]=4)[CH2:8][O:9][C@H:3]12
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 284Formic AcidHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 516920Potassium bisulfateHCID 1317350904-[2-[[(3R,3aR,6R,6aR)-3-hydroxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-6-yl]oxy]-6-chloro-1-(2-trimethylsilylethoxymethyl)-imidazo[4,5-b]pyridin-5-yl]benzonitrile

生成物 1

HCID 90042535
4-[2-[[(3R,3aR,6R,6aR)-3-hydroxy-2,3,3a,5,6,6a-hexahydro-furo[3,2-b]furan-6-yl]oxy]-6-chloro-1H-imidazo[4,5-b]pyridin-5-yl]benzonitrile

反応条件

温度
40 °C

実験手順

A flask was charged with 4-[2-[[(3R,3aR,6R,6aR)-3-hydroxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-6-yl]oxy]-6-chloro-1-(2-trimethylsilylethoxymethyl)-imidazo[4,5-b]pyridin-5-yl]benzonitrile (209.8 mg, 0.397 mmol), formic acid (3.6 ml, 94 mmol), and saturated aqueous KHSO4 (0.4 ml). The reaction mixture was heated to 40° C. for 16 h. Then the reaction mixture was cooled to room temperature before being cooled to 0° C. in an ice bath. A 50% weight solution of aqueous NaOH (5.3 ml, 200.7 mmol) was added to the reaction mixture, which solidified after being removed from the ice bath and was allowed to warm to room temperature. The reaction mixture was diluted with THF (2.0 ml) and water (10.0 ml) to give a hazy biphasic mixture with a pH of 14 that was stirred at room temperature for 30 min. The pH was adjusted to 5 by the addition of 2 N aqueous HCl. The reaction mixture was partitioned between EtOAc (50 ml) and water (20 ml). The aqueous layer was extracted with EtOAc (2×50 ml). The organic layers were combined, washed with brine (1×30 ml), dried over Na2SO4, filtered, and evaporated under reduced pressure to give a light pink residue. This material was purified by preparative HPLC reverse phase (C-18), using a 30×150 mm Sunfire™ column and eluting with a 20%-100% acetonitrile/water+0.05% TFA gradient, followed by a 100% acetonitrile+0.05% TFA flush. The product fractions were combined, evaporated under reduced pressure, and lyophilized from ethanol and benzene to give the title compound as a white solid. LC-MS: calculated for C19H15ClN4O4 398.08 observed m/e: 399.09 (M+H)+ (Rt 1.07/2 min); 1H NMR δ (ppm) (CD3OD): 7.84 (s, 1H), 7.84 (qt, J=8.3 Hz, 4H), 5.54 (qt, J=5.3 Hz, 1H), 4.96 (t, J=5.2 Hz, 1H), 4.46 (t, J=5.0 Hz, 1H), 4.25-4.30 (m, 1H), 4.16 (dd, J=5.6 Hz, J=10.2, 1H), 4.11 (dd, J=4.7 Hz, J=10.2 Hz, 1H), 3.89 (dd, J=7.0 Hz, J=8.1 Hz, 1H), 3.59 (t, J=8.6 Hz, 1H).

後処理

  1. temperatureThen the reaction mixture was cooled to room temperature
  2. temperaturebefore being cooled to 0° C. in an ice bath
  3. customafter being removed from the ice bath
  4. temperatureto warm to room temperature
  5. additionThe reaction mixture was diluted with THF (2.0 ml) and water (10.0 ml)
  6. customto give a hazy biphasic mixture with a pH of 14 that
  7. customThe reaction mixture was partitioned between EtOAc (50 ml) and water (20 ml)
  8. extractionThe aqueous layer was extracted with EtOAc (2×50 ml)
  9. washwashed with brine (1×30 ml)
  10. dry with materialdried over Na2SO4
  11. filtrationfiltered
  12. customevaporated under reduced pressure
  13. customto give a light pink residue
  14. customThis material was purified by preparative HPLC reverse phase (C-18)
  15. washeluting with a 20%-100% acetonitrile/water+0.05% TFA gradient
  16. customflush
  17. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-952b5104670b4867b85642750fc6e792
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09290517B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート