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Sodium hydride → HCID 67981025、化合物

HRID 1520063
ノート
印刷プレビュー

反応式

HRID 1520063 の反応式
[H-].[Na+].[F:3][C:4]1[CH:5]=[C:6]([C:11]2[CH:12]=[CH:13][C:14](=[O:17])[NH:15][N:16]=2)[CH:7]=[C:8]([F:10])[CH:9]=1.Br[CH2:19][C:20]1[CH:21]=[C:22]2[C:26](=[CH:27][CH:28]=1)[N:25](C(OC(C)(C)C)=O)[N:24]=[C:23]2[C:36]1[N:37]=[N:38][N:39]([C:41]2[CH:46]=[CH:45][C:44]([C:47]([O:49]C)=[O:48])=[CH:43][CH:42]=2)[CH:40]=1.C([O-])(O)=O.[Na+]>CN(C=O)C.[OH-].[Na+].CS(C)=O>[F:3][C:4]1[CH:5]=[C:6]([C:11]2[CH:12]=[CH:13][C:14](=[O:17])[N:15]([CH2:19][C:20]3[CH:21]=[C:22]4[C:26](=[CH:27][CH:28]=3)[NH:25][N:24]=[C:23]4[C:36]3[N:37]=[N:38][N:39]([C:41]4[CH:46]=[CH:45][C:44]([C:47]([OH:49])=[O:48])=[CH:43][CH:42]=4)[CH:40]=3)[N:16]=2)[CH:7]=[C:8]([F:10])[CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 24758Sodium hydrideHCID 516892Sodium Bicarbonate2 回HCID 252417496-(3,5-difluorophenyl)-2H-pyridazin-3-oneHCID 67981095tert-butyl 5-(bromomethyl)-3-{1-[4-(methoxycarbonyl)phenyl]-1H-1,2,3-triazol-4-yl}-1H-indazole-1-carboxylate

生成物 1

HCID 67981025HCID 67981025、化合物収率 109.2%

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 6228Dimethylformamide溶媒2 回HCID 14798Sodium Hydroxide溶媒

実験手順

Sodium hydride (34. mg; 0.78 mmol; 2.0 eq.) was added in one portion to a solution of 6-(3,5-Difluoro-phenyl)-2H-pyridazin-3-one (106 mg; 0.51 mmol; 1.3 eq.) in DMF (3 mL). After 10 min a solution of tert-butyl 5-(bromomethyl)-3-{1-[4-(methoxycarbonyl)phenyl]-1H-1,2,3-triazol-4-yl}-1H-indazole-1-carboxylate (392 mg; 0.38 mmol; 1.0 eq.) in DMF (3 mL) was added dropwise over 2 min and the reaction solution stirred for 4 h at RT. The reaction mixture was then poured into saturated solution of NaHCO3 and extracted with EtOAc. Combined organic phases were dried over magnesium sulfate, filtered and concentrated to give a yellow solid. This solid was redissolved in NaOH (5N, 0.5 mL) and DMSO (2 mL) and heated in MW for 10 min at 80° C. Reaction mixture was poured in a saturated solution of NaHCO3 and washed with EtOAc. The basic aqueous phase was acidified to pH 1 with 1N HCl and extracted with EtOAc. Combined organic phases were washed with brine, dried over magnesium sulfate, filtered and concentrated to give the title compound as a yellow solid (218 mg, 100%). 1H NMR (300 MHz, DMSO-d6) δ 13.43 (s, 1H), 9.44 (s, 1H), 8.47 (s, 1H), 8.29-8.09 (m, 6H), 7.68 (d, J=7.2 Hz, 2H), 7.63-7.47 (m, 2H), 7.40-7.30 (m, 1H), 7.14 (d, J=9.8 Hz, 1H), 5.52 (s, 2H). HPLC (Condition A): Rt 3.87 min (purity 52.8%). MS (ESI+): 526.2, MS (ESI−): 524.2.

後処理

  1. extractionextracted with EtOAc
  2. dry with materialCombined organic phases were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto give a yellow solid
  6. customReaction mixture
  7. washwashed with EtOAc
  8. extractionextracted with EtOAc
  9. washCombined organic phases were washed with brine
  10. dry with materialdried over magnesium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated

出典と根拠

ORDレコード
ord-eba8eab6e62647f497ccc43a361d784a
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09073892B2

反応ノート

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